Author: Jessica.F

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. 15205-15-9, name is 2-Chloro-6-fluorobenzylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 2-Chloro-6-fluorobenzylamine

(0.14 mmol, 31.9 mg) was dissolved in 1 mL of dimethyl sulfoxide (DMSO), to which were added HOBt (0.35 mmol, 49.43 mg), EDCI ¡¤ HCl (0.35 mmol, 68.42 mg), DIEA (0.56 mmol, 73.79 mg). After stirring at room temperature for 15 minutes, (0.14 mmol, 22.82 mg) was added. The reaction was carried out at room temperature for 5 hours. The reaction system was extracted with water/ethyl acetate (3 x 15 mL), then the organic phase was washed with saturated sodium chloride solution, dried with anhydrous sodium sulfate, concentrated, purified by reverse phase preparative HPLC (using 0.35% trifluoroacetic acid-containing aqueous solution and methanol as mobile phase), and vacuum concentrated to obtain compound III-f-1 (15.3 mg, 29.6%).

The synthetic route of 15205-15-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xiamen University; DENG, Xianming; WANG, Hongrui; ZENG, Taoling; ZHANG, Ting; JIANG, Tingting; (181 pag.)EP3626718; (2020); A1;,
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Application of 26487-67-2, 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. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 11: Synthesis of (4-(methylthio)phenyl)(naphthalen-l-yl)methanone 0-2-(azepan-l-yl)ethyl oxime oxalate (Compound 5h). Into a 50 ml round bottom flask, 4-(methylthio)phenyl (naphthalen-l-yl)methanone oxime (1 mmole, 293 mg), l-(2-Chloro-ethyl)-azepane hydrochloride (1.2 mmole, 237.6 mg), baked K2CO3 (5 mmole, 690 mg) and dry acetone (10.0 ml) were taken. The reaction mixture was refluxed under anhydrous conditions for 6 hours. The reaction was followed by TLC monitoring. After completion of the reaction, 2CO3 was filtered off and washed with acetone (2×10 ml). Filtrate was concentrated and the crude product was purified by basic alumina column chromatography using distilled Hexane to yield the pure product (350mg, 83.7percent). The product obtained was oily so a salt of the compound was prepared. Procedure for oxalate salt formation: Oxalic acid, 1 mmole/ 1 mmole of compound, (105.5 mg) and oily product (350 mg) were dissolved in dry methanol separately into two round bottom flasks. The acid and the compound were mixed and shaken thoroughly. The salt was precipitated using dry diethyl ether, filtered, washed with the same and collected. Yield: 427 mg, 78.49percent. M.P. (Oxalate Salt of compound) =145¡ã C; ESI MS(m/z)= 419 (M+H); ); IR(KBr, Cm-1): 3444.7, 2931.2, 2604.7, 1921.2, 1741.9, 1430.3, 1246.1, 1095.6, 1066.0, 961.0, 777.3; NMR(300MHz, CDCI3): delta= 7.93(d, J=8.2 Hz, 2H, ArH), 7.68(d, J=8.2 Hz, 1H, ArH), 7.58-7.39(m, 5H, ArH), 7.33-7.28(m, 1H, ArH), 7.18(d, J=8.6 Hz, 2H, ArH), 4.28(t, J=6.1 Hz, 2H, OCH2), 2.78(t, J=.5 Hz, 2H, NCH2), 2.51(m,. 4H, NCH2), 2.47(s, 3H, SCH3), 1.49(m, 8H, CH2); Analysis Calculated for C26H30N2OS (free base): C, 74.60; H, 7.22; N, 6.69, found: C, 74.62; H, 7.20; N, 6.68.

The chemical industry reduces the impact on the environment during synthesis 1-(2-Chloroethyl)azepane hydrochloride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH; SANYAL, Sabyasachi; KUMAR, Atul; CHATTOPADHYAY, Naibedya; LAL, Jawahar; TRIVEDI, Arun Kumar; DATTA, Dipak; RATH, Srikanta Kumar; AKHTAR, Tahseen; DWIVEDI, Shailendra Kumar Dhar; YADAV, Manisha; CHAKRAVARTI, Bandana; SINGH, Abhishek Kumar; MISHRA, Jay Sharan; SINGH, Nidhi; TRIPATHI, Anil Kumar; WO2015/29068; (2015); A1;,
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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 3972-56-3 as follows. name: 1-tert-Butyl-4-chlorobenzene

100 ml of 60% nitric acid was added dropwise to 100 ml of 95% sulfuric acid, at a temperature of 35C or less, under ice-cooling, to prepare a mixed acid solution. 100 g (0.593 mol) of 4-tert-butylchlorobenzene (A-1) was added dropwise to this mixed acid solution, at a temperature of 30C or less, followed by after-reaction (20 to 25C) for 2.5 hours. The reaction solution was poured into cold water, and it was then extracted with 100 ml of toluene, followed by washing with water, to obtain a toluene solution of (A-2).

According to the analysis of related databases, 3972-56-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; FUJI PHOTO FILM CO., LTD.; EP1535898; (2005); A1;,
Chloride – Wikipedia,
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Reference of 41965-95-1, 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 41965-95-1 as follows.

In a flask, tetrahydrofuran (4.5 L) was added, 3-chloro-4-methoxybenzylamine hydrochloride (500 g, 2.4 mol) was added under stirring, triethylamine (836 mL, 6.01 mol) was added dropwise, the mixture was stirred at room temperature for 30 min, cooled with ice-water, then ethyl 4-chloro-2-methylthiopyrimidine-5-carboxylate (466 g, 2.0 mol) was added, the reaction was stirred overnight at room temperature. TLC was used to monitor the reaction. After the end of reaction, solvent was removed by evaporation under reduced pressure. Ethyl acetate (2.5 L) and water (1 L) were added, the mixed liquid phases were separated, the organic phase was sequentially washed with diluted hydrochloric acid, water (1 L), saturated sodium bicarbonate (1 L) and saturated sodium chloride (1 L), dried over anhydrous sodium sulfate. After filtration, solvent was removed by evaporation under reduced pressure to obtain an oily substance, to which was added methanol (3 L), and a large white solid was precipitated. After stirring for 30 min, filtration was carried out, and the filter cake was vacuum dried to obtain the product (650 g, yield of 88.3%).

According to the analysis of related databases, 41965-95-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; XUANZHU PHARMA CO., LTD.; Shu, Chutian; Wu, Yongqian; (34 pag.)US2016/46654; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

771583-81-4, name is 4-Chloro-2-(trifluoromethyl)benzylamine, 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: C8H7ClF3N

4-((4- (ethylsulfonyl) benzyl) carbamoyl) benzoic acid (100.0 mg, 0.29 mmol), HATU (164.2 mg, 0.43 mmol) and DIPEA (185.7 mg, 1.44 mmol) were dissolved in tetrahydrofuran ( 5 mL), after stirring at room temperature for 0.5 hours, 4-chloro-2-trifluoromethylbenzylamine (60.6 mg, 0.29 mmol) was added, and the mixture was reacted at room temperature for 4 hours, and then an appropriate amount of water was added, followed by extraction with ethyl acetate. 3 times. The organic phases were combined and washed with a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated. The concentrate was purified by preparative high performance liquid chromatography to obtain the title compound (80.0 mg, yield: 51%).

The synthetic route of 771583-81-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan Kelun Botai Bio-pharmaceutical Co., Ltd.; Liu Chunchi; Liu Jinming; Cai Jiaqiang; Wang Lichun; Wang Jingyi; (25 pag.)CN110724076; (2020); A;,
Chloride – Wikipedia,
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Application of 56961-77-4,Some common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, 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.

29.3 g (100.0 mmol) of Compound 1-A, 22.6 g (100.0 mmol) of Compound 1-B, 2.7 g (3.0 mmol) of Pd2(dba)3, 1.3 g (6.0 mmol) of PtBu3 (50% solution in toluene), 28.8 g (300.0 mmol) of NaOtBu were mixed with 1,500 mL of toluene under a nitrogen (N2) atmosphere, followed by stirring under reflux to allow a reaction to occur for 12 hours. At room temperature, an organic layer was separated therefrom using water and ethyl acetate, and the solvent was dried. Then, through silica gel column chromatography, 28.5 g of compound 49-C was obtained at a yield of 65%. [0352] MS (MALDI-TOF) m/z: 438 [M]+

The synthetic route of 56961-77-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung Display Co., Ltd.; KIM, Myeongsuk; YE, Jimyoung; YOO, Byeongwook; JEONG, Jaeho; (102 pag.)US2020/98991; (2020); A1;,
Chloride – Wikipedia,
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These common heterocyclic compound, 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, 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: 63624-28-2

General procedure: To a mechanically stirred suspension of suspension of 1 (0.21 g, 0.53 mmol) in 30 ml CH2Cl2 were added triethylamine (0.5 ml) and aromatic sulfonyl chloride (0.53 mmol) at 25 C for 4 h. The reaction process was detected by TLC method. Then, antagonized by dilute sodium hydroxide, extracted, and washed with ether and water, evaporated under vacuum. Finally, the mixture was recrys-tallizated from ethyl acetate , providing a total product yield of 65.4%-88.6 %.

The synthetic route of 2,4-Dimethoxybenzene-1-sulfonyl chloride has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang; Aili; Zhang; Xu; Pharmazie; vol. 74; 2; (2019); p. 73 – 78;,
Chloride – Wikipedia,
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Related Products of 97329-43-6, A common heterocyclic compound, 97329-43-6, name is 1-Bromo-2-chloro-3-methylbenzene, molecular formula is C7H6BrCl, 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.

Preparation of l-(2-chloro-3-methylphenyl)propan-2-one: A Smith process vial was charged with l-bromo-2-chloro-3 -methylbenzene (528 mg, 2.57 mmol, 1 eq.), tributylmethoxytin (1.11 mL, 1.5 eq.), 4-methylpent-4-en-2-one (0.42 mL, 1.5 eq.), PdCl2 (23 mg, 5%) and tri(o-tolyl)phosphine (79 mg, 10%), toluene (1 mL) was added and mixture sparged with nitrogen for 10 minutes and then heated in oil bath at 100 C for 5 hours. The reaction mixture was diluted with ethyl acetate and washed with brine, dried (MgS04), filtered, concentrated and purified by flash column chromatography (silica gel, 0 to 20% ethyl acetate/hexanes) to l -(2-chloro-3-methylphenyl)propan-2- one (375 mg, 80% yield). 1H-NMR: 400 MHz, (CDC13) delta : 7.19-7.02 (m, 3H), 3.82(s, 2H), 2.38(s, 3H), 2.18 (s, 3H).

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; GILEAD SCIENCES, INC.; BABAOGLU, Kerim; BJORNSON, Kyla; GUO, Hongyan; HALCOMB, Randall, L.; LINK, John, O.; MCFADDEN, Ryan; MITCHELL, Michael, L.; ROETHLE, Paul; TRENKLE, James, D.; VIVIAN, Randall, W.; XU, Lianhong; WO2012/3497; (2012); A1;,
Chloride – Wikipedia,
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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. 1005-56-7, name is O-Phenyl carbonochloridothioate, A new synthetic method of this compound is introduced below., Safety of O-Phenyl carbonochloridothioate

General procedure: Phenyl chlorothionoformate (345 mg, 2.0 mmol), amine 2 (4.0 mmol) and water (15 mL) were added successively to a 50 mL round-bottom flask. The reaction mixture was stirred at room temperature for 1 h (monitored by TLC). After the reaction was complete, the solid was filtered off, washed with 10% HCl (2 ¡Á 20 mL) and deionised water(2 ¡Á 20 mL), and dried under vacuum to give the pure thiocarbamates 3. All products are known compounds and were identified by comparison of their physical and spectral data with those reported inthe literature.28

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:
Article; Li, Zhengyi; Chen, Yuan; Yin, Yue; Wang, Zhiming; Sun, Xiaoqiang; Journal of Chemical Research; vol. 40; 11; (2016); p. 670 – 673;,
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Application of 50594-82-6, These common heterocyclic compound, 50594-82-6, name is 3,4,5-Trichlorobenzotrifluoride, 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.

STR73 12.5 g (0.05 mol) of 3,4,5-trichloro-benzotrifluoride are added slowly and with stirring to a mixture of 8.0 g (0.05 mol) of 2,7-dihydroxynaphthalene, 4.2 g (0.075 mol) of pulverulent potassium hydroxide and 100 ml of dimethyl sulphoxide, which has been warmed to 60 C., and the reaction mixture is then stirred for a further approx. 3 hours at 60 C. After the mixture has been cooled to approximately 20 C., it is diluted with water and methylene chloride, and filtered. The organic phase is separated off from the filtrate, washed with water, dried using sodium sulphate and filtered. The solvent is removed from the filtrate by distillation in a water-pump vacuum, the residue is stirred with petroleum ether and the product which is thus obtained in the form of crystals is isolated by filtering with suction. 4.9 g (26% of theory) of 7-(2,6-dichloro-4-trifluoromethylphenoxy)-2-naphthol of melting point 98 C. are obtained. In analogy to Example (II-1) the starting substances of the formula (II) listed below in Table 2 may be prepared. STR74

The synthetic route of 50594-82-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bayer Aktiengesellschaft; US5041609; (1991); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics