Month: July 2021

13745-86-3, name is 11-Chlorodibenzo[b,f][1,4]thiazepine, 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. Application In Synthesis of 11-Chlorodibenzo[b,f][1,4]thiazepine

(b) 11-Piperazinyl-dibenzo[b,f][1,4]thiazepine. Piperazine (1.7 mole) was dissolved in warm toluene (about 50C.) (750 ml) and 11-chloro-dibenzo[b,f][1,4]thiazepine was added. The reaction was heated to reflux and maintained at this temperature for 5 hours. After cooling to ambient temperature the reaction was filtered to remove piperazine hydrochloride, and the organic phase was washed several times with water to remove excess piperazine. The organic phase was dried over magnesium sulfate and after filtration the solvent was removed in vacuo to give the product as an oil. The oil was dissolved in ethanol and treated with a solution of hydrogen chloride in ethanol. 11-Piperazinyl-dibenzo[b,f][1,4]thiazepine was isolated as the dihydrochloride salt in about 88% yield.

The synthetic route of 13745-86-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ICI Americas Inc.; US4879288; (1989); A;,
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. 694-80-4, name is 1-Bromo-2-chlorobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1-Bromo-2-chlorobenzene

1L three bottles,To a solution of 32.5 g of 2,4,6-triisopropylbromobenzene,5.6 g of magnesium turnings and 300 mL of anhydrous THF,20 g of o-chlorobromobenzene was dropwise added,2,4,6-triisopropyl-2-bromobiphenyl Grignard reagent,Refluxed for 2 hours,Down to room temperature,2.4 g of tetrakis (triphenylphosphine) palladium was added,Stirred for 30 minutes,18.8 g of di-tert-butylphosphonium chloride was added dropwise at room temperature,The reaction was refluxed for 5 hours.And the mixture was added dropwise to the reaction solution under ice-water bath200 mL of saturated aqueous ammonium chloride was quenched,Liquid separation,The organic phase is dissolved,Add methanol crystallization,And filtered to obtain 41.7 g of white 2-di-tert-butylphosphine-2,4,6-triisopropylbiphenyl,Yield 94%.

The synthetic route of 694-80-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Panjin Gelin Kaimo Technology Co., Ltd.; Rao, Zhihua; Gong, Ningrui; (12 pag.)CN105859774; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 15205-11-5, A common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, molecular formula is C7H7ClFN, 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.

Example 281-[(2-Chloro-4-fluorophenyl)methyl]-4-(4-fluoro-2,6-dimethylphenyl)-2,3- piperazinedione (E28)Methyl [(4-fluoro-2,6-dimethylphenyl)(2-oxoethyl)amino](oxo)acetate (0.15 g, 0.49 mmol) was dissolved in dichloromethane (5 ml) and cooled to O0C. 4 Angstrom molecular seives (0.3 g, 0.49 mmol), acetic acid (0.09 ml, 1.48 mmol), 2-chloro-4- fluorobenzylamine (0.07 ml, 0.54 mmol) and sodium triacetoxyborohydride (0.16 g, 0.74 mmol) were added. After 5 minutes, the reaction was warmed to room temperature and stirred for 16 hours overnight. Saturated aqueous sodium bicarbonate (5 ml) was added and the mixture stirred for 10 minutes. The organic layer was separated using a hydrophobic frit and concentrated in vacuo. The crude material was purified by mass-directed automated HPLC to yield 1-[(2-chloro-4- fluorophenyl)methyl]-4-(4-fluoro-2,6-dimethylphenyl)-2,3-piperazinedione (0.083 g) as a white solid. LC/MS [M+H]+ = 379, retention time = 2.84 minutes.

The synthetic route of 15205-11-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; CHAMBERS, Laura Jane; DEAN, David Kenneth; MUNOZ-MURIEDAS, Jorge; STEADMAN, Jon Graham Anthony; WALTER, Daryl Simon; WO2010/125103; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 14862-52-3, A common heterocyclic compound, 14862-52-3, name is 3,5-Dibromochlorobenzene, molecular formula is C6H3Br2Cl, 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 the round bottom flask was charged with 1,3-dibromo-5-chlorobenzene, 25g (92.47mmol) and 31.3g (184.9mmol) of diphenylamine , into a sodium t- butoxide 26.7g (277.41mmol) was added to 463ml toluene dissolved. Here Pd (dba)2 0.266g (0.462mmol) and tri-tert-butylphosphine was put 0.187g (0.924mmol) in turn and the mixture was stirred under reflux for 4 hours under a nitrogen atmosphere. After the reaction the organic layer was then extracted with ethyl acteate dry distilled over magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The product n- hexane / dichloromethane (9: 1 by volume) to yield the silica gel column 34.7g (84% yield) was purified by chromatography to the desired compound of intermediate M-10 as a white solid.

The synthetic route of 14862-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chei Industries Inc.; Ryu, Dong Wan; Heo, Dal Ho; Jung, Seong Hyeon; Hong, Jin Seok; Kim, Jun Seok; Yoo, Dong Kyu; Lee, Seung Jae; Lee, Han Il; Chang, Yu Na; Cho, Yeong Kyeong; Chae, Mi Yeong; (44 pag.)KR2016/8651; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 883499-24-9, 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. 883499-24-9, name is 1-Bromo-2-chloro-3-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a nitrogen atmosphere, a flask containing 1-bromo-2-chloro-3-fluorobenzene (10.4 g, 1 eq.), 1OH3NP11D (21.3 g, 50 eq., 1 eq.), potassium carbonate (13.7 g, 2 eq.), and NMP (100 ml) was heated and stirred at 180 C. The reaction liquid was cooled to room temperature, and NMP was distilled off under reduced pressure. Subsequently, water and toluene were added thereto, and the mixture was partitioned. Subsequently, the resulting product was purified by silica gel column chromatography (developing liquid: toluene/heptane=1/1 (volume ratio)), and thus ?1 Br2CL3Px(3NP11D)? was obtained.

The synthetic route of 1-Bromo-2-chloro-3-fluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kwansei Gakuin Educational Foundation; JNC Corporation; HATAKEYAMA, Takuji; KONDO, Yasuhiro; NAKAMOTO, Keiichi; YANAI, Motoki; (190 pag.)US2018/94000; (2018); 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. 81927-55-1, name is Benzyl 2,2,2-trichloroacetimidate, A new synthetic method of this compound is introduced below., Recommanded Product: Benzyl 2,2,2-trichloroacetimidate

[0484] To a solution of Scheme 5-8 compound SI (24 g, 0.136 mol) and benzyl 2,2,2- trichloroacetimidate (51.3 g, 0.204 mol) in cychexane/dichloromethane (600 mL/120 ml.,) at room temperature was added trifJuoromethanesuifonic anhydride (cat. 1.2 mL) dropwise. The reaction mixture was stirred at room temperature overnight, and filtered. The filtrate was washed with sat. NaHCCb, brine, dried over anhydrous Nay.SO-i, filtered and concentrated. The residue was purified by column chromatography on silica gel (eluted with petroleum ether: ethyl acetate 10. 1 ) to afford the title compound (35 g, 93.3% yield) as a yellow oil .

The synthetic route of 81927-55-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WILES, Jason, Allan; PHADKE, Avinash, S.; DESHPANDE, Milind; AGARWAL, Atul; CHEN, Dawei; GADHACHANDA, Venkat, Rao; HASHIMOTO, Akihiro; PAIS, Godwin; WANG, Qiuping; WANG, Xiangzhu; GREENLEE, William; (325 pag.)WO2017/35405; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 60811-21-4, 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. 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A mixture of a fluorinated aryl halide (2.0 mmol), a carbazole (0.5 mmol), and a base (2.0 mmol) in solvent (2 mL) was allowed to react under air atmosphere. The reaction mixture was heated to the specified temperature for 24 h. After reaction completion, the mixture was added to brine (15 mL) and extracted with CH2Cl2 (3 × 15 mL). The combined extract was concentrated under reduced pressure and the product was isolated by short chromatography on a silica gel (200-300 mesh) column.

The chemical industry reduces the impact on the environment during synthesis 4-Bromo-2-chloro-1-fluorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Wang, Lei; Ji, Enhui; Liu, Ning; Dai, Bin; Synthesis; vol. 48; 5; (2016); p. 737 – 750;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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. SDS of cas: 2533-69-9

Step 1-Synthesis of 4-[6-bromo-2-(trichloromethyl)-1,3-benzodiazol-1-yl]pyrimidin-2-amine To a solution of 4-N-(2-amino-5-bromophenyl)pyrimidine-2,4-diamine (3.0 g, 10.71 mmol) in acetic acid (10 mL) was added methyl 2,2,2-trichloroethanimidoate (1.4 mL, 11.25 mmol). The reaction was stirred at 45 C. for 7 hr. Water (15 mL) was then added. The precipitate was collected by filtration and dried under vacuum to give the title product (3.94 g as the acetic acid salt); 1H NMR (500 MHz, DMSO) delta 1.90 (3H, s), 7.01 (1H, d, J=5.0 Hz), 7.21 (2H, s), 7.75-7.46 (2H, m), 8.09-7.75 (1H, m), 8.58 (1H, d, J=5.0 Hz); LC-MS: m/z=+406/408/410/412 (M+H)+.

The synthetic route of Methyl 2,2,2-trichloroacetimidate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Genentech, Inc.; US2012/214762; (2012); 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. 622-86-6, name is (2-Chloroethoxy)benzene, A new synthetic method of this compound is introduced below., SDS of cas: 622-86-6

Example 29 N-2-(4-(2-phenoxyethoxy)-phenyl)-propyl-2-propanesulfonamide. To a stirred mixture of N-tertbutoxyacetyl-2-(4-hydroxyphenyl)propyl-2-propanesulfonamide (0.250 g,.70 mmol) in dry dimethylformamide (4 mL) was added sodium hydride (0.062 g, 0.87 mmol) under nitrogen. The resulting mixture was stirred 30 minutes at ambient temperature or until hydrogen gas evolution had ceased. Next, beta-chlorophenetole (0.120 g, 0.77 mmol) and sodium iodide (0.042 g, 0.25 mmol) are added and the resulting mixture was heated to 65C for 12 h. The resulting mixture was cooled and partitioned between ethyl acetate and water. The organic layer was washed with water (2 X 20 mL) and brine (1 X 20 mL), dried over magnesium sulfate, and filtered. Evaporation of the filtrate in vacuo followed by chromatography on silica gel eluding with ethyl acetate-hexane gave 0.250 g (75%) of the protected sulfonamide. To a stirred mixture of dichloromethane: trifluoroacetic acid (2 mL, 1:1) was added the protected sulfonamde (0.220 g, 0.42 mmol) under nitrogen. The resulting mixture was stirred at ambient temperature for 4 h. The mixture was partitioned between dichloromethane and 10% aqueous potassium carbonate. The organic layer was washed with brine (1 X 20 mL), dried over magnesium sulfate, and filtered. Evaporation of the filtrate in vacuo gives 0.166 g (96%) of the pure title compound. Mass Spectrum: MS +1= 378.5

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; ELI LILLY AND COMPANY; EP994110; (2000); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 4584-46-7 as follows. Application In Synthesis of 2-Chloro-N,N-dimethylethanamine hydrochloride

Caesium carbonate (3.0 Eq), sodium iodide (0.14 Eq) and 2-chloro-N,N- dimethylethylamine hydrochloride (1.5 Eq) are added to a suspension of p-bromo-phenol (1.0 Eq) in butanone (50 mL). The suspension is kept under reflux for four hours, after which the solid is filtered through a Hirsch funnel and washed with acetone, and the solvent is evaporated at low pressure. The crude product (yellow oil) is purified by silica-gel chromatography (eluent: dichloromethane-methanol; 95:5) to obtain the desired product (2-p-bromophenoxyethyl-N,N-dimethylamine) as a colourless oil (yield 70%).

According to the analysis of related databases, 4584-46-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UNIVERSITA’ DEGLI STUDI DI MILANO; FUMAGALLI, Laura; PICOZZI, Claudia; REGAZZONI, Luca; CARINI, Marina; ALDINI, Giancarlo; VISTOLI, Giulio; (26 pag.)WO2019/53626; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics