Category: chlorides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, 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 13918-92-8, Recommanded Product: 13918-92-8

a) N-[5 -bromo-2-(methyloxy)-3-pyridinyl] -2,4-difluorobenzenesulfonamide. To a cooled (0 0C) solution of 5-bromo-2-(methyloxy)-3-pyridinamine (100 mmol) in pyridine (200 rnL) was added slowly 2,4-difluorobenzenesulfonyl chloride (100 mmol) over 15 min (reaction became heterogeneous). The ice bath was removed and the mixture was stirred at ambient temperature for 16 h, at which time the reaction was diluted with water (500 mL) and the solids filtered off and washed with copious amounts of water. The precipitate was dried in a vacuum oven at 500C to give the title product as an ivory solid (32 % yield). MS(ES) m/e 380.9, 379.0 (M + H)+.

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, 2,4-Difluorobenzene-1-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2009/39140; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 15205-11-5, These common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, 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 91 N-[(2-chloro-4-fluorophenyl)methyl]-5-oxo-1-phenyl-prolinamide (E91) 5-oxo-1-phenyl-proline (0.072 g, 0.35 mmol, prepared as described below) was dissolved in dichloromethane (~2 ml) and dimethylformamide (0.5 ml) and to this was added N-(3-dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride (0.081 g, 0.42 mmol), 1-hydroxybenzotriazole (0.057 g, 0.42 mmol), and N-ethyl morpholine (0.134 ml, 1.05 mmol). The mixture was stirred at room temperature for 30 minutes and then [(2-chloro-4-fluorophenyl)methyl]amine (0.067 g, 0.42 mmol) was added. Stirring was continued overnight at room temperature and then the mixture was diluted with more dichloromethane and saturated aqueous sodium hydrogen carbonate. The aqueous layer was separated and extracted with more dichloromethane (3 aliquots). The combined organic layers were then washed with brine before drying over magnesium sulphate. Evaporation of the solvent then gave a yellow oil which was purified by mass-directed automated HPLC. Finally trituration of the material thus obtained with a 1:1 mixture of dichloromethane and diethyl ether gave, after filtration and drying, pure N-[(2-chloro-4-fluorophenyl)methyl]-5-oxo-1-phenyl-prolinamide (0.031 g) as a white solid. LC/MS [M+H]+=347, retention time=2.46 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; US2008/9541; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1939-99-7, A common heterocyclic compound, 1939-99-7, name is Phenylmethanesulfonyl chloride, molecular formula is C7H7ClO2S, 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.

A solution of phenylmethanesulfonyl chloride (2.19 g, 10 mmol) was added into a suspension of 3-bromopropan-l-amine hydrobromide (2.19 g, 10 mmol) and Et3N (2.02 g, 20 mmol) in THF (50 mL) at 0 C. The mixture was stirred at 0 C for 5 min. TLC confirmed the completion of reaction. Solid was filtered out with suction, and the filtrate was concentrated to provide compound N-(3- bromopropyl)(phenyl)methanesulfonamide (2.7 g, quant.) as a pale yellow solid which was used in the next step without further purification. lU NMR (300 MHz, CDC13) delta 7.40 (m, 5H), 4.48 (m, 1H), 4.27 (s, 2H), 3.41 (t, J = 6.6 Hz, 2H), 3.16 (q, 2H), 2.01 (m, 2H). LCMS (ESI), m/z, 314 and 316 [M+Na]+, Br pattern found.

The synthetic route of 1939-99-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; FAUBER, Benjamin; GANCIA, Emanuela; LADDUWAHETTY, Tammy; VESEY, David; WINSHIP, Paul; RENE, Olivier; (168 pag.)WO2017/5900; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 367-22-6,Some common heterocyclic compound, 367-22-6, name is 4-Chloro-3-fluoroaniline, molecular formula is C6H5ClFN, 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: Compound 7 (488.2 mg, 2.0 mmol), 3,4-dimethoxybenzenamine 8a (367.6 mg, 2.4 mmol), and p-toluenesulfonic acid monohydrate (304.4 mg, 1.6 mmol) were dissolved in n-butanol (20 mL), then refluxed at 130 oC for 12 h. The resulting solution was neutralized with saturated NaHCO3 (5 mL). The mixture was extracted with ethyl acetate (50 mL×3). The organic layer was combined, dried over anhydrous Na2SO4, concentrated. The crude product was purified by silica gel chromatography to afford 9a (319.7 mg, 44.3% yield).

The synthetic route of 367-22-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Long, Liang; Luo, Yu; Hou, Zhi-Jie; Ma, Hua-Juan; Long, Zi-Jie; Tu, Zheng-Chao; Huang, Lin-Jie; Liu, Quentin; Lu, Gui; European Journal of Medicinal Chemistry; vol. 145; (2018); p. 805 – 812;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 932-96-7, 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. 932-96-7, name is 4-Chloro-N-methylaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

4-Chloro-N-methylaniline (1.6 mL, 12.9 mmol) in toluene (44 mL) was added to a mixture of Cs2CO3 (4.9 g, 15.05 mmol), Pd(OAc)2 (0.121 g, 0.538 mmol), BINAP (0.502 g, 0.806 mmol) and 5-bromopicolinaldehyde (2.00 g, 10.75 mmol). The mixture was stirred at 85 C. for 15 h and after cooling filtered through Celite. The solids were washed with EtOAc. The combined filtrates were concentrated and the residue purified by chromatography to give the sub-title compound. Yield: 1.537 g (58%).

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, 4-Chloro-N-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nilsson, Peter; Pelcman, Benjamin; Katkevics, Martins; Ronn, Robert; Krog-Jensen, Christian; US2013/35358; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, molecular formula is CH4Cl2N2, 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: 29671-92-9

2-Amino-5-chloro-3,9-dihydro-4H-pyrimido[4,5-b]indol-4-one (8) 1 g methyl sulfone was heated to melting. 7 (106.22 mg, 1.37 mmol) was added and the resulting mixture was stirred and heated at 110-120 C. to dissolve completely. 5 (200 mg, 0.837 mmol) was added in one part to the reaction mixture. Stirring was continued for 30 minutes. About 10 mL water was added to quench the reaction. Ammonia water was added to neutralize the reaction mixture. Solid precipitated out. This solid was filtered. Obtained solid was dissolved in chloroform and methanol, dried (using Na2SO4) and recrystallized.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 29671-92-9, its application will become more common.

Reference:
Patent; Gangjee, Aleem; US2009/62318; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 6781-98-2, name is 2-Chloro-1,3-dimethylbenzene, 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-1,3-dimethylbenzene

General procedure: To a 50 mL Schlenk tube containing base (1.5 mmol) and precatalyst 4a (1 mol percent, 0.0083 g) purged with N2 (three times), amine (1.2 mmol) was added via syringe, and the resulted mixture was allowed to stir at room temperature for 2?3 min. Solvent (1 mL) was then injected via syringe followed by the aryl chloride (1.0 mmol). If the aryl chloride was a solid, it was introduced into the vial prior to purging with N2. At this time, the reaction was stirred for 24 h at 100 °C. After cooling to the room temperature, the reaction mixture was concentrated in vacuo and directly purified via silica gel flash chromatography. 2,6-Dimethyl-N-(o-tolyl)aniline (17) ;1H NMR (CDCl3, 400 MHz, 298 K): delta=7.28-7.22 (m, 4H), 7.15-7.05 (m, 1H), 6.88-6.80 (m, 1H), 6.33-6.25 (m, 1H), 5.04 (br s, 1H), 2.46 (s, 3H), 2.33 (s, 6H); 13C NMR (CDCl3, 100 MHz, 298 K): delta=114.05, 138.67, 135.46, 130.18, 128.48, 126.86, 125.48, 122.32, 118.03, 111.64, 18.16, 17.58.

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

Reference:
Article; Fang, Weiwei; Jiang, Jian; Xu, Yong; Zhou, Juefei; Tu, Tao; Tetrahedron; vol. 69; 2; (2013); p. 673 – 679;,
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, Recommanded Product: 2533-69-9

In an ice-water bath, compound 39 (307 mg, 1.75 mmol) was slowly added dropwise to a solution of compound 41 (500 mg, 1.46 mmol) in acetic acid (50 mL).After stirring at room temperature for 3 hours, it was concentrated under reduced pressure.The residue was washed with a saturated sodium bicarbonate solution,After extraction with ethyl acetate, it was purified through a silica gel column (PE / EA = 5/1 to 1/1) to obtain Intermediate 14 (600 mg) as a white solid.

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; Shanghai Meiyue Bio-technology Co., Ltd.; Hu Zhilong; Feng Yan; Wang Xiaolin; Li Shiqiang; Yu Shanghai; Ding Yawen; Dai Feihong; He Qian; Wang Chaodong; (44 pag.)CN110343089; (2019); 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. 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, A new synthetic method of this compound is introduced below., Recommanded Product: Sodium 4-chlorobenzenesulfinate

A 1-propanol (50 ml) solution of 4-chloromethylpyridine hydrochloride (1.26 g, 7.65 mmol), sodium 4-chlorobenzenesulfinate (1.52 g, 7.65 mmol) and potassium acetate (1.50 g, 15.3 mmol) was stirred under heating at 70C for 8 hours. The reaction mixture was cooled to room temperature and then concentrated under reduced pressure. The residue thus obtained was caused to pass through a short column (silica gel, ethyl acetate) and the eluate was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography, and the fraction obtained from the hexane:ethyl acetate (=2:3) eluate was concentrated under reduced pressure to give the title compound (1.26 g, 62%) as a white solid. 1H-NMR(400MHz, CDCl3) delta: 4.29(2H,s), 7.06(2H,d,J=6.1Hz), 7.47(2H,d,J=8.8Hz), 7.59(2H,d,J=8.5Hz), 8.57(2H,d,J=6.1Hz). MS (m/z) : 268 (M++H).

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; DAIICHI PHARMACEUTICAL CO., LTD.; EP1640366; (2006); A1;,
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. 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 6579-54-0

2.6-Dichlorobenzenesulfonyl chloride (100 mg, 0.41 mmol) was dissolved in DCM (0.5 mL) and triethylamine (0.11 mL, 0.81 mmol) was added followed by 2- [2- (trifluoromethyl)phenyl]ethanamine (0.11 mL, 0.69 mmol). The reaction mixture was stirred for 2 hours at room temperature. DCM (10 mL) and brine (10 mL) were added to the mixture. The layers were separated and the organic phase was dried over magnesium sulfate, filtered and the solvent was evaporated. Purification by column chromatography on silica gel with petroleum ether/DCM (60:40 to 40:60) afforded the title compound as white solid (131 mg, 80 %). MS ESI+ m/z 398 [M+H]+.

The synthetic route of 6579-54-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLUCOX BIOTECH AB; WIKSTROeM, Per; WALUM, Erik; (126 pag.)WO2019/215291; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics