The important role of 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide

The synthetic route of 4090-55-5 has been constantly updated, and we look forward to future research findings.

4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C5H10ClO3P

In a reflux condenser, thermometer, stirrer,Constant pressure dropping funnel 2000mL four-necked flask was added 74g of cyclic phosphorus oxychloride,8 g of anhydrous aluminum trichloride and 800 mL of toluene were added to dissolve them with stirring.Under stirring at 10 C,22.8gBetween cyclohexane diamine four-necked flask,After the addition of cyclohexane diamine is completed,The temperature was raised to 80 C,And the reaction at this temperature 6h, after the reaction was recovered by vacuum distillation solvent,The residue was washed three times with deionized water to give a white solid powder,After drying at 60 C for 10 h, 73.3 g of a product was obtained in a yield of 89.8% by weight.

The synthetic route of 4090-55-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sinopec Corporation; Sinopec Corporation Fushun Petrochemical Institute; Zhao Wei; Wang Xiaolin; Li Ming; Liu Mingrui; Xue Qian; (8 pag.)CN104558039; (2017); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Simple exploration of 4090-55-5

The synthetic route of 4090-55-5 has been constantly updated, and we look forward to future research findings.

4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C5H10ClO3P

In a 250-mL three-necked flask with a flux condenser, thermometer, a mechanical stirrer and dropping funnel, neopentyl glycol (20.8 g, 0.2 mol) and chloroform (100 mL) were mixed. After the solids were dissolved completely in ice-water bath, 39.8 g (0.26 mol) of phosphorus oxychloride was then slowly dropped into the above reaction vessel within 2 h, and then, the temperature of the mixtures was increased to refluxing temperature for 4 h. After that, the solvent was removed by a rotary evaporator; then, the white powders were obtained (intermediate II) [17]. The schematic processes for the reactions are presented in Scheme 1(a). The intermediate II 73.8 g (0.4 mol) and acetonitrile (300 mL) were added into a three-necked flask with an ice bath equipped with a mechanical stirrer, flux condenser, dropping funnel and drying tube with calcium chloride. Then, 35.0 g of 9,9-bis (4-hydroxyphenyl)fluorene (0.1 mol) was added to the mixtures and the mixtures were kept stirring in the ice-water bath. Triethylamine (1.5 mL) was then slowly dropped into the above reactants, and the temperatures of the mixtures were increased to 60 C for another 10 h. After that, the acetonitrile was removed by rotary evaporator and the white products were obtained. The white products were washed by distilled water and further recrystallized from distilled water and ethyl alcohol for two times. Then, the white products were obtained (49.46 g, 76.6%). The schematic processes of the reaction are presented in Scheme 1(b). 1H NMR: 7.742-6.662 ppm, -C6H2- in the benzene ring; 4.252-3.957 ppm, OCH2; 1.325, 0.918, 1.325 and 0.918 ppm -CH3. MS: [M + K]+ = 687.4; thus, the molecular weight of the FRs is 648.4.

The synthetic route of 4090-55-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Qian, Xiaodong; Guo, Nan; Zhao, Yanhua; Lu, Lingang; Wang, Huiya; Wang, Xuebao; Jin, Jing; Shao, Gaosong; Hu, Zhijia; Journal of Thermal Analysis and Calorimetry; vol. 131; 3; (2018); p. 2625 – 2636;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

New learning discoveries about C5H10ClO3P

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 4090-55-5, HPLC of Formula: C5H10ClO3P

Synthesis Example 1 (Synthesis of Phosphorus Compound 1) (Reaction); In a four-necked 1-L flask provided with a stirrer, a thermometer, a dropping device, a hydrochloric-acid-absorber device and a condenser, 104.0 g (1 mole) of neopentyl glycol and 114.4 g of chlorobenzene were fed. The resulting mixture was heated at 45 to 55 C while stirring and 153.5 g (1 mole) of phosphorus oxychloride were dropwise added to the mixture in an hour. After addition, the mixture was heated to 75 C in an hour, and then was allowed to react at the same temperature (75 C) for an hour and 65.7 g of generated hydrogen chloride were recovered. Thereafter, the mixture was depressurized at the same temperature (75 C) and 26.6 kPa for 2 hours and remaining hydrogen chloride was absorbed as a gas. As a result, 298.9 g of the reaction mixture were obtained. The purity of the reaction mixture was found to be 95.6 area % by GPC (gel permeation chromatography). The resulting reaction mixture was cooled to room temperature to which 161.5 g (0.95 mole) of 2-phenylphenol (ortho-phenylphenol), 0.9 g of magnesium chloride and 145.6 g of chlorobenzene were added. The mixture was heated at 65 to 75 C while stirring and 106.1 g (1.05 moles) of triethylamine were dropwise added to the mixture in an hour. Thereafter, the mixture was allowed to react at the same temperature (75 C) for an hour and thereby obtaining a mixture of 5, 5-dimethyl-2-(2′-phenylphenoxy)-1, 3, 2-dioxaphosphorinane-2-oxide.(After-treatment) The obtained mixture was neutralized at 85 C by adding hydrochloric acid solution which corresponds to an excess amount of triethylamine and the mixture was allowed to stand to separate an oil phase. Next, the obtained oil phase was washed with approximately 85 C water and then dehydrated. The obtained oil phase was gradually cooled and 259.8 g of white needle-like crystals were crystallized out from the oil phase. The purity of the obtained crystals was found to be 99.0 area % by GPC. Also, if all of the crystals were assumed to be an object compound, the crude yield was 86.0 %. A structure of the obtained crystals was determined according to results of quantitative analysis of phosphorus by elemental analysis and absorption spectrometry using an UV spectrometer, 1H-NMR, 13C-NMR and FT-IR. The crystals were identified as 5, 5-dimethyl-2-(2′-phenylphenoxy)-1, 3, 2-dioxaphosphorinane-2-oxide (phosphorus compound 1) of the below-mentioned constructional formula. Also, a melting point of the crystal was measured by a microdose melting point apparatus (model number: MP-J3, manufactured by Yanaco Co., Ltd.). Quantitative analysis of phosphorus by elemental analysis and absorption spectrometry (theoretical values in parentheses): Carbon: 64.3 % (64.2 %) Hydrogen: 5.9 % (6.0 %) Phosphorus: 9.7 % (9.7 %) Melting point: 127 to 130 CIR (KBr): 2992, 2352, 1584, 1514, 1485, 1430, 1373, 1306, 1251, 1104, 1158, 1120, 1050, 1004, 980, 947, 922, 877, 701, 624 cm-1 2992, 2352, 1584, 1514, 1485, 1430, 1373, 1306, 1251, 1104, 1158, 1120, 1050, 1004, 980, 947, 922, 877, 701, 624 cm-1 NMR: 1H-NMR (CDCl3; 300MHz); delta 7.71 (1H, d, J=8Hz, o-PP), 7.55-7.26 (8H, m, o-PP), 3.62 (1H, d, J=10Hz, POCH2C(CH3)2-), 3.53 (2H, dd, JHH=10Hz, POCH2C(CH3)2-), 3.48 (1H, d, JHH=10Hz, POCH2C(CH3)2-), 1.17 (3H, s, POCH2C(CH3)2-), 0.42 (3H, s, POCH2C(CH3)2-) ppm1H-NMR (CDCl3; 300MHz); delta 7.71 (1H, d, J=8Hz, o-PP), 7.55-7.26 (8H, m, o-PP), 3.62 (1H, d, J=10Hz, POCH2C(CH3)2-), 3.53 (2H, dd, JHH=10Hz, POCH2C(CH3)2-), 3.48 (1H, d, JHH=10Hz, POCH2C(CH3)2-), 1.17 (3H, s, POCH2C(CH3)2-), 0.42 (3H, s, POCH2C(CH3)2-) ppm13C-NMR (CDCl3; 75MHz); delta 146.9 (d, 2JPC=6Hz), 137.3, 132.7 (d, 3JPC=7Hz), 130.9, 129.6, 129.0, 128.2, 127.6, 125.2, 120.4 (d, 3JPC=2Hz) (o-PP), 77.6 (d, 2JPC=7Hz, POCH2C(CH3)2-), 31.5 (d, 2JPC=6Hz, POCH2C (CH3)2-), 21.6, 19.5 ppm

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, and friends who are interested can also refer to it.

Reference:
Patent; DAIHACHI CHEMICAL INDUSTRY CO., LTD.; EP1925622; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Simple exploration of 4090-55-5

The synthetic route of 4090-55-5 has been constantly updated, and we look forward to future research findings.

Electric Literature of 4090-55-5,Some common heterocyclic compound, 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, molecular formula is C5H10ClO3P, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a one-liter four-necked flask equipped with a stirrer, a thermometer, a thermostat, a dropping device (funnel), a hydrochloric-acid-recovering device (condenser connected with a water scrubber) and a reflux condenser, 226.8 g (0.9 moles) of dibutyl(1-hydroxy-1-methylethyl)phosphonate as an alcohol compound, 111.1 g (1.1 moles) of triethylamine as a hydrogen halide scavenger, 1.14 g (0.012 moles) of magnesium chloride as a catalyst and 20.8 g of toluene as an organic solvent were put in and stirred. The resulting mixed solution was retained at a temperature of 60C by using the thermostat, and the whole amount of each solution synthesized in Examples and Comparative Examples was added thereto gradually over 2 hours by using the dropping device. After completion of the addition, the resulting reaction mixture was stirred at a temperature of 60C for 1 hour to complete the reaction. Subsequently, 200 g of water was added to the resulting reaction mixture. The resulting solution was stirred at a temperature of 60C for 30 minutes, and then was allowed to stand to be separated into phases. Then, an aqueous phase was recovered to remove triethylamine hydrochloride generated as a by-product. Subsequently, 3.0 g (0.02 moles) of a 30% aqueous sodium hydroxide was added to the reaction mixture. The resulting solution was retained at a temperature of 20 to 60C by using the thermostat, and 97.1 g of a 35% hydrogen peroxide aqueous solution (1.0 mole as hydrogen peroxide) was added thereto gradually over 2 hours by using the dropping device. After completion of the addition, the resulting reaction mixture was stirred at a temperature of 60C for 1 hour to complete the reaction. Then, the resulting reaction mixture was washed with an aqueous hydrochloric acid solution and a sodium carbonate aqueous solution sequentially, and finally rinsed with water. The resulting reaction mixture was heated to a temperature of 100 to 140C, and the pressure was reduced to 100 torr (13.3 kPa) to recover water and toluene. Further, steam distillation was performed at a temperature of 100 to 140C under a reduced pressure of 20 torr (2.7 kPa) to remove low-boiling point components to obtain a transparent and colorless liquid (compound 1). The liquid obtained was analyzed by gas chromatography, and the result thereof was compared with gas chromatographic analysis results of cyclic phosphoric acid esters having known cyclic structures to confirm that the main component of the liquid obtained was each of the following cyclic phosphoric acid esters.

The synthetic route of 4090-55-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daihachi Chemical Industry Co., Ltd.; EP2495247; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some tips on 4090-55-5

The synthetic route of 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Safety of 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide

General procedure: Ph(But)P(O)Cl or 2-chloro-5,5-dimethyl-1,3,2-dioxaphosphinane 2-oxide (5.0mmol) was added to the suspension of NaH (0.133g, 5.5mmol) in THF (25mL). Subsequently, 5,7-dibromo-2-methylquinolin-8-ol (1a), 5-fluoro-2-methylquinolin-8-ol (1i) (5.0mmol) in THF (5mL), was added. The reaction was carried out for 24 h under reflux. The mixture was allowed to cool to room temperature. The reaction was neutralized with aqueous solution of KHSO4. After extraction with CH2Cl2 (3¡Á50mL), the organic phase was dried over MgSO4, followed by filtration and solvent evaporation. The crude product was purified by chromatography and crystallization.

The synthetic route of 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide has been constantly updated, and we look forward to future research findings.

Reference:
Article; Nycz, Jacek E.; Szala, Marcin; Malecki, Grzegorz J.; Nowak, Maria; Kusz, Joachim; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 117; (2014); p. 351 – 359;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some tips on 4090-55-5

Statistics shows that 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide is playing an increasingly important role. we look forward to future research findings about 4090-55-5.

Application of 4090-55-5, These common heterocyclic compound, 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

The NCS was synthesized according to the literature (Kang and Li 2004). In a 250mL three-necked round-bottomed ask equipped with a magnetic stirrer and a reux condenser, PCL 18.40g (0.10mol) and acetonitrile (100mL) were mixed at 65C. Then, potassium thiocyanate 24.20g (0.25mol) was feed into the ask by batch addition, and the mixture was stirred at 65C for 8h. After the reaction, mixture was cooled slowly to room temperature, ltered, and evaporated under vacuum. A red mixture was obtained and washed with dichloromethane (30mL) to remove residual sylvite, ltered, and evaporated under vacuum. Repeat the post-processing process twice, an orange-red oily liquid was collected, and which was named as NCS, and the yield was 95%.

Statistics shows that 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide is playing an increasingly important role. we look forward to future research findings about 4090-55-5.

Reference:
Article; You, Ge-Yun; He, Hong-Wu; Feng, Bin; Tang, Yu-Ying; Cheng, Zhi-Quan; Fan, Fang-Fang; Chemical Papers; vol. 74; 8; (2020); p. 2403 – 2414;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

The origin of a common compound about 4090-55-5

According to the analysis of related databases, 4090-55-5, the application of this compound in the production field has become more and more popular.

Application of 4090-55-5, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 4090-55-5 as follows.

(Synthesis of phosphorus compound (1)); The flask accommodating the post-reaction solution containing intermediate 2 was filled with 121. 4 g (1.2 mol) of triethylamine, 1.85 g (0.015 mol) of 4-(dimethylamino) pyridine, and 420 g of 1, 2-dichloroethane. While the mixed solution was stirred, a mixed solution of 177.1 g (0.96 mol) of material 1 and 450 g of 1,2-dichloroethane was added thereto at 20C over 2 hours. After that, the substances were reacted at the same temperature (20C) for 8 hours. The obtained post-reaction solution was neutralized at room temperature using an aqueous solution of hydrochloric acid in an amount corresponding to the excess amount of triethylamine. The resultant solution was kept still so as to be separated into different layers. Then, the organic layer was neutralized using an aqueous solution of sodium hydrogen carbonate. The organic layer was then washed with water twice. The obtained organic layer was dried by anhydrous magnesium sulfate. Toluene was added to the filtrate, and recrystallization was performed. Thus, 171. 4 g of phosphorus compound (1) was obtained. Phosphorus compound (1) had a purity measured by GPC (gel permeation chromatography) of 100% by area. The yield was 54.4%.

According to the analysis of related databases, 4090-55-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DAIHACHI CHEMICAL INDUSTRY CO., LTD.; EP1632497; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Extracurricular laboratory: Synthetic route of 4090-55-5

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 4090-55-5, Formula: C5H10ClO3P

Synthesis Example 3 (Synthesis of Phosphorus Compound 3); A mixture was obtained in the same manner as in Synthesis example 1 except that 114.4 g of toluene were used in place of 114.4 g of chlorobenzene, 161.5 g of 4-phenylphenol (para-phenylphenol) (0.95 mole) were used in place of 161.5 g of 2-phenylphenol (ortho-phenylphenol) (0.95 mole) and 127.5 g of toluene were used in place of 145.6 g of chlorobenzene to add to the reaction mixture.(After-treatment) The obtained mixture was cooled to room temperature and neutralized by adding a hydrochloric acid solution which corresponds to an excess amount of triethylamine, and allowed to stand to separate an oil phase. Next, the obtained oil phase was washed with approximately 85 C water and then any liquid was removed by a centrifugal filter. The obtained solid was dried by a vacuum desiccator at 100 C, to give 253.7 g of a white solid. The purity of the obtained solid was found to be 98.7 area % by GPC. Also, if all of the solids were assumed to be an object compound, the crude yield was 84.0 %. A structure of the obtained solid was determined according to results of quantitative analysis of phosphorus by elemental analysis and absorption spectrometry using an UV spectrometer, 1H-NMR, 13C-NMR and FT-IR, and the solid was identified as 5, 5-dimethyl-2-(4′-phenylphenoxy)-1, 3, 2-dioxaphosphorinane-2-oxide (phosphorus compound 3) of the below-mentioned constructional formula. Also, a melting point of the solid was measured in the same manner as in Synthesis example 1. Quantitative analysis of phosphorus by elemental analysis and absorption spectrometry (theoretical values in parentheses): Carbon: 64.3 % (64.2 %) Hydrogen: 6.1 % (6.0 %) Phosphorus: 9.7 % (9.7 %) Melting point: 165 to 167 CIR (KBr): 3008, 1606, 1523, 1488, 1405, 1376, 1296, 1226, 1194, 1174, 1114, 1059, 1002, 934, 861, 810, 765, 720, 691, 624 cm-1 3008, 1606, 1523, 1488, 1405, 1376, 1296, 1226, 1194, 1174, 1114, 1059, 1002, 934, 861, 810, 765, 720, 691, 624 cm-1 NMR: 1H-NMR (CDC13; 300MHz); delta 7.57-7.31 (9H, m, o-PP), 4.27 (2H, d, JHH=11Hz, POCH2C (CH3)2-), 4.01 (2H, dd, JHH=11Hz, JPH=22Hz, POCH2C (CH3)2-), 1.34 (3H, s, POCH2C (CH3)2-), 0.92 (3H, s, POCH2C (CH3)2-) ppm1H-NMR (CDC13; 300MHz); delta 7.57-7.31 (9H, m, o-PP), 4.27 (2H, d, JHH=11Hz, POCH2C (CH3)2-), 4.01 (2H, dd, JHH=11Hz, JPH=22Hz, POCH2C (CH3)2-), 1.34 (3H, s, POCH2C (CH3)2-), 0.92 (3H, s, POCH2C (CH3)2-) ppm13C-NMR (CDC13; 75MHz); delta 149.7 (d, 2JPC=6Hz), 140.0, 138.1, 128.7, 128.4, 127.2, 126.9, 119.7 (d, 3JPC=5Hz) (o-PP), 78.3 (d, 2JPC=7Hz, POCH2C (CH3)2-), 32.1 (d, 2JPC=6Hz, POCH2C (CH3)2-), 21.6, 20.1 ppm

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DAIHACHI CHEMICAL INDUSTRY CO., LTD.; EP1925622; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Share a compound : 4090-55-5

According to the analysis of related databases, 4090-55-5, the application of this compound in the production field has become more and more popular.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 4090-55-5

The flask accommodating the post-reaction solution containing intermediate 4 was filled with 121.4 g (1.2 mol) of triethylamine and 1.85 g (0.015 mol) of 4-(dimethylamino) pyridine. While the mixed solution was stirred, a mixed solution of 164.2 g (0.89 mol) of material 1 and 450 g of toluene was added thereto at 20C over 2 hours. After that, the substances were reacted at the same temperature (20C) for 8 hours. The obtained post-reaction solution was neutralized at room temperature using an aqueous solution of hydrochloric acid in an amount corresponding to the excess amount of triethylamine. The resultant solution was kept still so as to be separated into different layers. Then, the organic layer was neutralized using an aqueous solution of sodium hydrogen carbonate. The organic layer was then washed with water twice. The obtained organic layer was dried by anhydrous magnesium sulfate. The solvent and water were removed by distillation, thereby obtaining 311.2 g of phosphorus compound (3). Phosphorus compound (3) had a purity measured by GPC (gel permeation chromatography) of 95.1% by area. The yield was 94.0%.

According to the analysis of related databases, 4090-55-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DAIHACHI CHEMICAL INDUSTRY CO., LTD.; EP1632497; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

The important role of 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide

According to the analysis of related databases, 4090-55-5, the application of this compound in the production field has become more and more popular.

4090-55-5, Adding a certain compound to certain chemical reactions, such as: 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 4090-55-5.

0.12 g of acid chloride IIIb in 2 mL of anhydrous benzene was added to 0.24 g of imine II and 0.08 g of triethylamine in 10 mL of anhydrous benzene upon stirring. The mixture was incubated during 12 h at room temperature. The precipitated triethylamine hydrochloride was separated,the solution was evaporated, and the residue was washed with diethyl ether. Yield 0.2 g (61%), mp 53-56C. IR spectrum (KBr), nu, cm-1: 1599 (Ph), 1623(C=N). 1H NMR spectrum, [(CD3)2CO], delta, ppm: 0.94 s(3H, CH3), 1.00 s (3H, CH3), 1.29 s (3H, CH3), 1.33 s (3H, CH3), 4.07-4.21 m (4H,OCH2), 4.44-4.60 m(4H, OCH2), 6.90-8.42 m (8H, Ph), 9.08 s (1H,PhCH). 31P NMR spectrum, [(CD3)2CO], deltap, ppm: 54.72, -21.57. Mass spectrum, m/z: 526. Found, %: C 52.34; H 5.39; N 2.94; P 11.99; S 5.69. C23H29NO7P2S. Calculated, %: C 52.56; H 5.57; N 2.67; P 11.79; S6.10.

According to the analysis of related databases, 4090-55-5, the application of this compound in the production field has become more and more popular.

Reference:
Letter; Bagautdinova; Burilov; Pudovik; Pudovik; Russian Journal of General Chemistry; vol. 85; 5; (2015); p. 1204 – 1206; Zh. Obshch. Khim.; vol. 85; 5; (2015); p. 875 – 876,2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics