Month: May 2021

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 19752-55-7 as follows. Product Details of 19752-55-7

In a 20 mL eggplant flask, 3,3′-bicarbazole,1-Bromo-3,5-dichlorobenzene, copper powder, potassium carbonate and nitrobenzene were charged, nitrogen bubbling was carried out for 1 hour, and the mixture was stirred at 170 C. for 17 hours under a nitrogen stream. Progress of the reaction was confirmed by TLC (ethyl acetate: hexane = 1: 3) to confirm disappearance of 3,3′-bicarbazole and cooled to room temperature. The reaction mixture was dissolved in chloroform and the insoluble matter was filtered through celite. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (chloroform: hexane = 1: 1) to obtain a pale yellow solid of BCzPhCl (yield: 810 mg, yield: 54%). It was identified by mass spectrometry (MS), 1 H-NMR. A chart of 1 H-NMR is shown in FIG. 2, and an enlarged view thereof is shown in FIG. 3. Table 1 shows the preparation conditions of this synthesis.A similar experiment is shown in Table 1Run No. 2

According to the analysis of related databases, 19752-55-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ChemiprokaseiCo., Ltd.; Kido Junji, Sasabe; Hisahiro, Naoki; Toyota, Naoki; Omae, Yoshinori; (110 pag.)JP5727237; (2015); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 2163-00-0, These common heterocyclic compound, 2163-00-0, name is 1,6-Dichlorohexane, 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.

Examples 2 to 5; The procedure of Example 1 was repeated, except that the reaction of 1,6-dichlorohexane was carried out at a constant pH of 5, 6, 8 and 9. Before the start of the particular reaction, the weakly acidic mixture was adjusted to the pH of 5, 6, 8 and 9 with 2.5% sodium hydroxide solution (measurement with pH electrodes). Example 2 Example 3 Example 4 Example 5 pH value in 5.0 +/- 0.1 6.0 +/- 0.1 8.0 +/- 0.1 9.0 +/- 0.1 the reaction Residual 1,6-dichloro- <10 <10 <10 approx. 11 hexane content (ppm) Conversion of 1,6- >99.9 >99.9 >99.9 >99.9 dichlorohexane (%) In all examples (Examples 2 to 5), the resulting reaction mixture was clear and homogeneous. To determine the pure yield with respect to Examples 2 and 5, they were repeated once more. However, a GC analysis sample was not taken from the particular reaction mixture. The pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate was approx. 91.4%2) for the repetition of Example 2 and approx. 90.6%2) for the repetition of Example 5. 2) The pure yield for the synthesis according to Examples 2 and 5 was carried out again as in Example 1 by reacting the reaction solutions obtained in each case with aqueous NaBEC solution. In this procedure, the yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was approx. 89.6% of theory with a content of 95% for the reaction according to Example 2 and approx. 89.7% of theory with a content of approx. 94% for that according to Example 5. Thus, the pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate in the inventive reaction of 1,6-dichlorohexane with sodium thiosulphate pentahydrate must have been approx. 91.4% for the reaction according to Example 2 (89.6%¡Á0.95¡Á1/0.931=91.4%) and approx. 90.6% for that according to Example 5 (89.7%¡Á0.94¡Á1/0.931=90.6%).

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Buding, Hartmuth; US2005/240044; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 699-89-8, name is 4,7-Dichlorothieno[2,3-d]pyridazine, A new synthetic method of this compound is introduced below., Recommanded Product: 699-89-8

Equal equivalents of dichloride (1) and M-NH2 are refluxed in the appropriate amount of absolute ethanol at 95 0C for 2 hrs. The reaction mixture is allowed to cool to room temperature and the precipitate (2) that forms is filtered and washed sequentially with isopropyl alcohol, 4.0 N KOH, H2O, and hexane, and then dried. The filtrate (2) is then reacted with 1.2 equivalent Of Q-NH2 in an appropriate amount of n-butyl alcohol at 150 0C for 10 hrs. The reaction is cooled to room temperature before the solvent is evaporated under reduced pressure. The residue is treated with aqueous 4.0 NKOH solution and extracted with dichloromethane. The organic layer is dried (MgSO4) and evaporated. The crude product (3) is purified by preparative thin layer chromatography (TLC) or flash chromatography on silica gel using dichloromethane/methanol (95:5) as the eluent. Final product is confirmed by LC/MS and/or nuMR. The invention compounds of Examples 23 – 25, 48, and 76-80 as shown in the below table were prepared by method A-I.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; BAYER HEALTHCARE AG; WO2007/118602; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 41965-95-1, 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. 41965-95-1 name is 3-Chloro-4-methoxybenzylamine Hydrochloride, 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.

To a heterogenous mixture of quinoline 13 (3.56 mmol) and 3-chloro-4- methoxy benzylamine-HCl (3.92 mmol) in NMP (15 mL) was added TNEt (8.90 mmol). The reaction mixture was heated to 80 C for 3 h. Subsequently, cooled the reaction mixture to ambient temperature and added 1M aqueous HQ and EtOAc. The resulting layers were separated and the organic layer washed with water (3x) followed by brine (1 x). The combined organic layers were dried over Na2S04, filtered, and concentrated in vacuo. The residue was dissolved in a minimum amount of hot EtOAc and allowed to cool to ambient temperature. Hexanes was then added to the solution and the intermediate 14 (80% yield) precipitated out and was collected by vacuum filtration. H NMR (300 MHz, CDCIj) 8 8.20 (s, 1 H), 7.95 (d, I H, , 7-8.4 Hz), 7.82 (d, 1 J=7.5 Hz), 7.38 is, IB), 7.27-7.22 im, 1 H), 6.98 (d, IR , 7-8.4 Hz), 6.26 (s, 1H), 4.54 (d. 2H J-4.8 Hz), 3.95 (s, 3H), 3.93 (s, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloro-4-methoxybenzylamine Hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; LANDRY, Donald, W.; DENG, Shixian; ARANCIO, Ottavio; FIORITO, Joie; WASMUTH, Andrew; WO2013/109738; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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 2533-69-9, COA of Formula: C3H4Cl3NO

EXAMPLE 2 The preparation of a mixture of 1,1′-bis(tridecyloxycarbonyl)-dimethyl-2,2′-bibenzimidazoles in which each benzene ring contains a methyl group in the 5- or 6-position. 3,4-Diaminotoluene (100.8 g) was dissolved in methanol (600 cm3) at room temperature. The solution was stirred while methyl 2,2,2-trichloroacetimidate (70.6 g) was added in a manner similar to that described in Example 1. The mixture was allowed to cool and was stirred at room temperature for 36 hours, then diluted with water (1.5 dm3) and filtered. The solid was added again to water (1 dm3) stirred at room temperature and filtered. The solid was added to aqueous 2N sodium carbonate solution (1 dm3) stirred at 70 C. for 12 hours, cooled and filtered. The solid was repeatedly washed with methanol (3*500 cm3) by slurrying and filtering to leave a pale tan coloured solid. This solid was treated with activated carbon, recrystallized from boiling dimethylformamide, and dried, yielding 49 g of 5,5′-dimethyl-2,2′-bibenzimidazole. By this method the free base rather than the monohydrochloride was isolated (found Cl<0.2%). The structure was confirmed by measurement of the proton NMR spectrum using a solution in trifluoracetic acid with tetramethylsilane as internal standard. 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, Methyl 2,2,2-trichloroacetimidate, other downstream synthetic routes, hurry up and to see. Reference:
Patent; Imperial Chemical Industries PLC; US5258524; (1993); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 6940-78-9, name is 1-Bromo-4-chlorobutane, 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 6940-78-9, Quality Control of 1-Bromo-4-chlorobutane

In a round bottom flask, 5.0 g of 7-hydroxyquinolin-2(1H)-one, 6.42 g K2CO3 and 25 ml acetone were taken and stirred for 30 minutes at 25-35 C. 5.89 g 1-bromo-4-chloro butane was added into the reaction mixture and stirred for 5-6 hours at 50-55 C. After completion of the reaction, the reaction mixture was cooled to 25-35 C. The reaction mixture was filtered. The solvent was removed by distillation under vacuum. The solid was dried in a hot air oven at 45-50 C. to obtain 7-(4-chlorobutoxy) quinolin-2(1H)-one. Yield: 85%.

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; CADILA HEALTHCARE LIMITED; DESAI, Sanjay Jagdish; PARIHAR, Jayprakash Ajitsingh; SHAH, Alpesh Pravinchandra; (21 pag.)US2017/320862; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-2-chloro-1-fluorobenzene

Example 112 Production of (4aS, 8aR)- 1 -(3 -chloro-4-fluoropheny l)-3 , 3 -dimethy ldecahydroquinoxaline hydrochloride bsolute configuration A toluene (10 ml) suspension of (4aR,8aS)-2,2-dimethyldecahydroquinoxaline (168 mg, 0.998 mmol), 4-bromo-2-chloro-l-fluorobenzene (251 mg, 1.20 mmol), Pd(OAc)2 (11.2 mg, 0.0500 mmol), t-Bu3P.HBF4 (14.5 mg, 0.0500 mmol), and NaOt-Bu (135 mg, 1.40 mmol) was stirred for 5 hours under reflux in a nitrogen atmosphere. The reaction solution was cooled to room temperature. Then, water (0.5 mL) and AcOEt (10 mL) were added thereto, and the mixture was stirred. MgS04 was further added thereto, and the mixture was stirred. Then, insoluble matter was filtered. The filtrate was concentrated under reduced pressure, and the obtained residue was purified by basic silica gel column chromatography (Hex- AcOEt). The obtained oil was dissolved in 1 N HCl-EtOH (3 mL), and ethanol was distilled off under reduced pressure. The deposited crystal was recrystallized from ethanol/acetone to obtain (4aS,8aR)-l- (3-chloro-4-fluorophenyl)-3,3-dimethyldecahydroquinoxaline hydrochloride (153 mg, yield: 46%) in a white powder form. 1H-NMR ( DMSO-de ) 6ppm : 1.15-1.45 ( 6H, m ), 1.51 ( 3H, s ), 1.6-1.9 ( 4H, m ), 1.9-2.05 ( 1H, m ), 2.94 ( 1H, d, J = 13.5Hz ), 3.3-3.45 ( lH, m ), 3.65-3.8 ( 1H, m ), 3.95-4.1 ( 1H, m ), 6.85-7.0 ( 1H, m ), 7.12 ( 1H, dd, J = 3.0, 6.2Hz ), 7.25 ( 1H, dd, J = 9.1, 9. lHz ), 8.13 ( 1H, br ), 9.86 ( 1H, br ).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; OTSUKA PHARMACEUTICAL CO., LTD.; SHINOHARA, Tomoichi; SASAKI, Hirofumi; TAI, Kuninori; ITO, Nobuaki; WO2013/137479; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 210532-25-5, 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. 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 3,5-difluorobenzenesulfonyl chloride (25 g, 0.117 mol) in THF (150 mL) was added 35% aq. NH4OH (120 mL) over 1 h in an ice-bath. After the reaction was complete, it was evaporated in vacuo. To a solution of this residue in water (150 mL) was added 2N HC1 (1 mL). After stirring 1 h, the reaction mixture was filtered and dried under high vacuum to give 3,5-difluorobenzenesulfonamide as a light brown solid (19.9 g, 88%). 1H NMR (400MHz, CDC13) delta 7.49-7.44 (m, 2H), 7.04-6.99 (m, 2H).

The chemical industry reduces the impact on the environment during synthesis 3,5-Difluorobenzene-1-sulfonyl chloride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; EXELIXIS, INC.; BOLLU, Venkataiah; BOREN, Brant, Clayton; DALGARD, Jackline; FLATT, Brenton, T.; HAQ, Nadia; HUDSON, Sarah; MOHAN, Raju; MORRISSEY, Michael; PRATT, Benjamin; WO2011/71565; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 13078-79-0, 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 13078-79-0 as follows.

Example S15; Preparation of (4-tert-butyl-benzyl)-[2-(3-chloro-phenyl)-ethyl]-amine; 0.38 ml of 4-tert-butylbenzaldehyde (2.25 mmol) and 0.215 ml 2-(3-chloro-phenyl)-ethylamine (1.5 mmol) were dissolved in 4.5 ml methanol at rt, and after stirring for 30 min at rt, were refluxed for 2.5 h. After cooling down to rt, 85 mg (2.25 mmol) sodium borohydride were added and after stirring for 5 min at rt, the reaction mixture was then refluxed for 4 h. After cooling down to rt, the reaction mixture was treated with 4 drops 1 N HCl and concentrated in vacuo. The residue was diluted with water/EtOAc. After separation of the organic phase, the aqueous phase was extracted with EtOAc and the combined organic phases were washed with brine, dried with magnesium sulfate, filtered off and concentrated in vacuo. The residue was purified by column chromatography (40 g silica gel; EtOAc/heptane 1:2) to give 465 mg light yellow oil (100%). MS (ISP) 302.3 (M+H)+.

According to the analysis of related databases, 13078-79-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Conte-Mayweg, Aurelia; Kuehne, Holger; Luebbers, Thomas; Maugeais, Cyrille; Mueller, Werner; Pflieger, Philippe; US2006/30613; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 303-49-1, name is 3-(3-Chloro-10,11-dihydro-5H-dibenzo[b,f]azepin-5-yl)-N,N-dimethylpropan-1-amine, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3-(3-Chloro-10,11-dihydro-5H-dibenzo[b,f]azepin-5-yl)-N,N-dimethylpropan-1-amine

Clomipramine 2 (0.503 g; 1.43 mmol; 1 equiv) was mixed with Cs2CO3 (1.13 g; 3.57 mmol; 2.5 equiv) and XPhos precatalyst PdG1 (0.0313 g; 0.0428 mmol; 3 mol %) in a glove box. To this anhydrous acetonitrile (4 mL) was added, and the reaction mixture was left with stirring, in the glove box for 25 min before THP protected propargyl alcohol (0.501 g; 3.57 mol; 2.5 equiv) was added. The reaction vessel was sealed, removed from the glove box, and then heated to 80 C for 20 h. After 20 h the reaction mixture was cooled to rt and quenched with saturated NaHCO3 (aq). The mixture was extracted with AcOEt, and the combined organic phases were dried over MgSO4, filtered and evaporated. The product was purified by column chromatography (first CH2Cl2/CH3OH 50:1 then CH2Cl2/CH3OH 20:1). Upon repeated column chromatography, the product was isolated as brown oil in 63% yield (0.375 g; 0.895 mmol). Rf (CH2Cl2/CH3OH 20:1) 0.45. 1H NMR (400 MHz, CDCl3) deltaH 7.16-7.02 (m, 4H), 6.99 (s, 2H), 6.94 (dt, 1H, J = 7.3, 1.1 Hz), 4.88 (t, 1H, J = 3.4 Hz) 4.46 (q, 2H, J = 15.7 Hz), 3.93-3.81 (m, 1H), 3.77 (t, 2H, J = 6.6 Hz), 3.61-3.50 (m, 1H), 3.12 (s, 4H), 2.60 (t, 2H, J = 5.6 Hz), 2.35 (s, 6H), 1.96-1.48 (m, 8H). 13C NMR (100 MHz, CDCl3) deltaC 147.9, 134.9, 134.4, 130.3, 129.7, 126.7, 125.9, 123.3, 123.2, 120.7, 120.4, 96.9, 86.0, 84.4, 62.1, 57.3, 54.9, 48.5, 44.9, 32.6, 31.8, 30.4, 25.5, 19.2 ppm. HRMS (ES+): Calcd for C27H34N2O2H: 419.2699; found 419.2699.

According to the analysis of related databases, 303-49-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Brink¡ã, Anne; Larsen, Maja T.; Kolds¡ã, Heidi; Besenbacher, Louise; Kolind, Anders; Schi¡ãtt, Birgit; Sinning, Steffen; Jensen, Henrik H.; Bioorganic and Medicinal Chemistry; vol. 24; 12; (2016); p. 2725 – 2738;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics