Category: 4090-55-5

Related Products 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

Related Products 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.

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 (3×50mL), the organic phase was dried over MgSO4, followed by filtration and solvent evaporation. The crude product was purified by chromatography and crystallization.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, its application will become more common.

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 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. Recommanded Product: 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide

(2R,3R,4R, 5R)-5 -((((((2R,3R,4R, 5R)-5-(6-Benzamido-9H-purin-9-yl)-4-((tert- butyldimethylsilyl)oxy)-2-(hydroxymethyl)tetrahydrofuran-3 -yl)oxy)(2-cyanoethoxy)phosphoryl)oxy)methyl)-4-((tert-butyldimethylsilyl)oxy)-2-(4-oxo-4, 5 -dihydro1 H-imidazo [4,5 -c]pyridin- 1 -yl)tetrahydrofuran-3 -yl hydrogen phosphonate (160 mg) was subjected to azeotropic dehydration with anhydrous pyridine, and anhydrous pyridine (3.0 mL) was added thereto. To the mixture was added 2-chloro-5,5-dimethyl-1,3,2- dioxaphosphinane 2-oxide (99 mg) at room temperature, and the mixture was stirred at room temperature for 1 hr. Water (96 1iL) and iodine (50.5 mg) were added thereto, and the mixture was stirred at room temperature for additional 20 mm. To the reaction mixture was added a mixture of sodium thiosulfate (190 mg) and water (0.4 mL), and the mixture was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methanol/ethyl acetate) to give the title compound (10.6 mg). MS: [M+H] 1044.3

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4090-55-5, its application will become more common.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; YOSHIKAWA, Masato; SAITOH, Morihisa; KATO, Taisuke; YOSHITOMI, Yayoi; SEKI, Tomohiro; NAKAGAWA, Yasuo; TOMINARI, Yusuke; SETO, Masaki; SASAKI, Yusuke; OKANIWA, Masanori; ODA, Tsuneo; SHIBUYA, Akito; HIDAKA, Kosuke; SHIOKAWA, Zenyu; MURATA, Shumpei; OKABE, Atsutoshi; NAKADA, Yoshihisa; MOCHIZUKI, Michiyo; FREEZE, Brian Scott; TAWARAISHI, Taisuke; WADA, Yasufumi; GREENSPAN, Paul D.; (423 pag.)WO2018/100558; (2018); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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, Recommanded Product: 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide

In a reflux condenser, thermometer, stirrer,Constant pressure dropping funnel 2000mL four-necked flask was added74g cyclic phosphorus oxychloride,8g anhydrous aluminum trichloride and800mL chloroform,Under stirring to make it fully dissolved.Under stirring at 10 C,22.8g of cyclohexanediamine was added to a four-necked flask,To be added after completion of cyclohexanediamine, the temperature was raised to 50 , and at this temperature for 8h,After the reaction was completed, the solvent was recovered by distillation under reduced pressure, the residue was washed with deionized water three times,A white solid powder was obtained, which was dried at 60 C for 10 h to give 72.5 g of the product in a yield of 88.8% by weight.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

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

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.

Synthesis Example 5 (Synthesis of Phosphorus Compound 7); 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, 137.0 g (0.95 mole) of 2-naphthol (beta-naphthol) were used in place of 161.5 g (0.95 mole) of 2-phenylphenol (ortho-phenylphenol) and chlorobenzene was not used to add to the reaction mixture.(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 any liquid was removed by a centrifugal filter. The obtained solid was dried by a vacuum desiccator at 100 C, to give 227.5 g of a white solid. The purity of the obtained solid was found to be 99.0 area % by GPC. Also, if all of the solids were assumed to be an object compound, the crude yield was 82.0 %. 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-(2′-naphthyloxy)-1, 3, 2-dioxaphosphorinane-2-oxide (phosphorus compound 7) 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: 61.6 % (61.6 %) Hydrogen: 5.9% (5.8 %) Phosphorus: 10.6 % (10.6%) Melting point: 151 to 155 CIR (KBr): 2992, 2896, 1632, 1600, 1513, 1466, 1374, 1357, 1306, 1251, 1210, 1171, 1123, 1053, 973, 938, 915, 867, 826, 784, 755, 675, 627 cm-1 2992, 2896, 1632, 1600, 1513, 1466, 1374, 1357, 1306, 1251, 1210, 1171, 1123, 1053, 973, 938, 915, 867, 826, 784, 755, 675, 627 cm-1 NMR: 1H-NMR (CDC13; 300MHz); delta 7.85-7.78 (3H, m, beta -Np), 7.72 (1H, s, beta-Np), 7.51-7.37 (m, 3H, beta-Np), 4.29 (2H, d, J=11Hz, POCH2C (CH3)2-), 4.01 (2H, dd, JHH= 11Hz, POCH2C (CH3)2-), 1.35 (3H, s, POCH2C (CH3)2-), 0.92 (3H, s, POCH2C (CH3)2-) ppm1H-NMR (CDC13; 300MHz); delta 7.85-7.78 (3H, m, beta -Np), 7.72 (1H, s, beta-Np), 7.51-7.37 (m, 3H, beta-Np), 4.29 (2H, d, J=11Hz, POCH2C (CH3)2-), 4.01 (2H, dd, JHH= 11Hz, POCH2C (CH3)2-), 1.35 (3H, s, POCH2C (CH3)2-), 0.92 (3H, s, POCH2C (CH3)2-) ppm13C-NMR (CDCl3; 75MHz); delta 147.8 (d, 2JPC=7Hz), 133.8, 130.8, 129.9, 127.6, 127.3, 126.7, 125.4, 119.4 (d, 3JPC=6Hz), 115.8 (d, 3JPC=5Hz) (o-PP), 78.3 (d, 2JPC=7Hz, POCH2C (CH3)2-), 32.1 (d, 2JPC=6Hz, POCH2C (CH3)2-), 21.6, 20.0 ppm

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, its application will become more common.

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

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.

(Synthesis of phosphorus compound (5)); The flask accommodating the post-reaction solution containing intermediate 6 was filled with 80.8 g (0.8 mol) of triethylamine, 4.1 g (0.034 mol) of 4-(dimethylamino) pyridine, and 420 g of 1, 2-dichloroethane. While the mixed solution was stirred, a mixed solution of 123.6 g (0 .67 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 and the amount of sodium methoxide used for synthesizing intermediate 6. 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 212.9 g of phosphorus compound (5). Phosphorus compound (5) had a purity measured by GPC (gel permeation chromatography) of 82.0% by area. The yield was 62.1%.

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

Related Products of 4090-55-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 4090-55-5 name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

BODIE was obtained by the reaction of ethylenediamine with DOPC in trichloromethane.The DOPC (193.79 g, 1. 05 mol) and triethylamine (151.79 g, 1.5 mol)mixture with trichloromethane (200 mL) was put into a dry, four-necked flask equipped asdescribed above. The ethylenediamine (30 g, 0.5 mol) dissolved in trichloromethane(50 mL) was added dropwise at 0-5 C. After the addition, the temperature was increasedslowly to the reflux temperature and then the reaction was stopped after refluxing for 4 h.The resulting white precipitate was filtered and washed with cold distilled water and thendried overnight. The white product (BODIE) was obtained with a yield of 94 %. The massfraction purity of BODIE is 99 % measured by HPLC.

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:
Article; Han, Feng; Pei, Liangjun; Xue, Fengfeng; Li, Dong; Journal of Solution Chemistry; vol. 45; 8; (2016); p. 1146 – 1157;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. HPLC of Formula: C5H10ClO3P

Comparative Synthesis Example 1 (Synthesis of Comparative Phosphorus Compound 1); 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, 89.3 g (0.95 mole) of phenol were used in place of 161.5 g (0.95 mole) of 2-phenylphenol (ortho-phenylphenol) and chlorobenzene was not used to add to the reaction mixture.(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 any liquid was removed by a centrifugal filter. The obtained solid was dried by a vacuum desiccator at 100 C, to give 210.0 g of a white solid. The purity of the obtained solid was found to be 99.2 area % by GPC. Also, if all of the solids were assumed to be an object compound, the crude yield was 86.8 %.

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

Reference 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.

In a 250 ml three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, 50 ml of acetonitrile, 2-aminothiazole (0.11 mol, 11.0 g) and triethylamine (0.3 mol, 30.3 g) were added and stirred to mix well. Further, a solution of neopentyl glycolphosphoryl chloride (0.1 mol, 18.5 g) in acetonitrile (100 ml) was added dropwise with stirring at 3 C, and the system remains clear and transparent. After the solution was added dropwise, the system was allowed to react at 3 C for 3 h, and then heated to 70 C for 8 h. After completion of the reaction, the solvent was removed by rotary evaporation to obtain a reddish brown solid, which was washed three times with chloroform to remove the triethylamine hydrochloride. After drying, a one-component intumescent flame retardant (PAZ) for epoxy resin was obtained. 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:
Patent; Fujian Normal University; Jian Rongkun; Ai Yuanfang; Xia Long; Pang Fuqu; (9 pag.)CN109400649; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: chlorides-buliding-blocks

Taking 0.01 muM structure 1 and 0.04 muM structure 3 by adding three-mouth flask, nitrogen protection, magnetic stirring dissolved in 200 ml dichloromethane in, ice water bath. In the slowly dripping triethylamine in three mouth bottle, during the dropping will be accompanied by white mist generating, heating up to 40 C, this temperature is kept continuous stirring 8 hours. The reaction liquid washing three times with saturated sodium chloride solution, adding anhydrous magnesium sulfate standing drying, after clarifying filtration, vacuum hangs steams to remove the solvent, to obtain orange crystal that aromatic module including cup and cyclic phosphate ester flame retardants, yield 85.39%.

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

Reference:
Patent; Chinese People’s Armed Police Force Academy; Lu Lingang; Wang Huiya; Qian Xiaodong; Yang Shousheng; Jin Jing; (8 pag.)CN107778328; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics