Month: March 2021

Application of 39226-96-5, 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. 39226-96-5, name is (2-Chloro-3-(trifluoromethyl)phenyl)methanamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Compound 2a (438mg, 2.5mmol) and 2-chloro-3-(trifluoromethyl)benzylamine (419mg, 2.0mmol) were mixed with EDAC (480mg, 2.5mmol) and 1-hydrobenzotrizole (HOBt, 338mg, 2.5mmol) in dry dichloromethane (60mL). The reaction mixture was stirred for overnight at RT. Then the resultant mixture was washed with 2N HCl (50mL) and saturated aqueous NaHCO3 (40mL). The organic layer was dried over Na2SO4 and concentrated. The residue was purified by column chromatography on silica gel with eluent (2:98 MeOH/CH2Cl2) to afford a white solid product 3a (210mg, 28%), Rf=0.34 (1:15 MeOH/CH2Cl2), mp 147-149C. 1H NMR (CDCl3): delta 2.03-2.09 (m, 1H, CH), 2.31-2.40 (m, 2H, CH2), 2.49-2.57 (m, 1H, CH), 3.21-3.30 (m, 1H, CH), 3.80 (dd, J=15.5, 36.0Hz, 1H, CH), 4.22 (dd, J=4.0, 8.0Hz, 1H, CH), 4.45-4.58 (m, 2H, CH2), 4.61 (d, J=6.0Hz, 2H, CH2Ph), 6.53 (br s, 1H, CONH), 7.37 (t, J=8.0Hz, 1H, Ph-H), 7.59 (d, J=8.0Hz, 1H, Ph-H), 7.66 (d, J=8.0Hz, 1H, Ph-H). 1C NMR (CDCl3): delta 23.96, 29.51, 41.92, 42.67 (d, JC-F=18.75Hz), 62.55 (d, JC-F=1.25Hz), 82.36 (d, JC-F=166.25Hz, CH2F), 119.66 (q, JC-F=271.25Hz, CF3), 127.11, 127.31 (q, JC-F=5.0Hz), 129.05 (q, JC-F=30.0Hz), 131.85, 133.92, 137.73, 171.51, 176.21. MS (ESI): 367 ([M+H]+, 100%); MS (ESI): 365 ([M-H]-, 50%). HRMS (ESI): calcd for C15H16N2O2ClF4 ([M+H]+) 367.0836, found 367.0848.

The synthetic route of (2-Chloro-3-(trifluoromethyl)phenyl)methanamine has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gao, Mingzhang; Wang, Min; Glick-Wilson, Barbara E.; Meyer, Jill A.; Peters, Jonathan S.; Territo, Paul R.; Green, Mark A.; Hutchins, Gary D.; Zarrinmayeh, Hamideh; Zheng, Qi-Huang; Bioorganic and Medicinal Chemistry Letters; vol. 28; 9; (2018); p. 1603 – 1609;,
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Reference of 1205-71-6, These common heterocyclic compound, 1205-71-6, name is 4-Chloro-N-phenylaniline, 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 round bottom flask, 8-bromobenzo [b] naphtho [2,1-d] thiophene (12 mmol), copper iodide (15 mmol), potassium tert-butoxide (65 mmol), 1,2-di Aminocyclohexane (12 mmol) and (12 mmol) (3-chloro-phenyl) -phenylamine were added to dry 1,4-dioxane (100 ml), and the mixture was refluxed under N2 atmosphere for 48 hours. The intermediate was cooled to room temperature, added to water, and then filtered through a pad of celite while extracting with dichloromethane, then washed with water, and dried over anhydrous magnesium sulfate. After filtration and evaporation, the crude product was purified by silica gel column chromatography to obtain Intermediate HT042-1.

Statistics shows that 4-Chloro-N-phenylaniline is playing an increasingly important role. we look forward to future research findings about 1205-71-6.

Reference:
Patent; Shanghai Tianma Organic Shine Display Co., Ltd.; Zhang Lei; Gao Wei; Niu Jinghua; Dai Wenpeng; Xiao Wenjing; Lu Yan; Zhu Hongyan; (28 pag.)CN110746391; (2020); A;,
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Related Products of 694-80-4, 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. 694-80-4, name is 1-Bromo-2-chlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of aryl silane (0.5 mmol), aryl bromides (0.5 mmol), PdCl2(MeCN)2 (5 mol%), and CsF (0.5 mmol) was stirred at 100oC for 6 h in NMP under CO (1atm) (5 mL). Afterwards, 2 mL water was added to the reaction solution and then filtered through a filter paper and the solution was extracted by Et2O (2 mL) for three times. The organic phase was combined and evaporated under reduced pressure. The residue was purified on a SiO2 column to afford the desired product(ethyl acetate/hexane).

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, 1-Bromo-2-chlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Chang, Sheng; Jin, Ying; Zhang, Xiu Rong; Sun, Yong Bing; Tetrahedron Letters; vol. 57; 19; (2016); p. 2017 – 2020;,
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Related Products of 61881-19-4, The chemical industry reduces the impact on the environment during synthesis 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, I believe this compound will play a more active role in future production and life.

General procedure: Add sodium acetate, trifluoroethylimidyl chloride (II), hydrazone (III), and 1 mL of organic solvent to the 35 mL Schlenk tube according to the raw material ratio in Table 1.Mix and stir well. After the reaction is completed according to the reaction conditions in Table 2, 2-4 hours,Add elemental iodine, continue the reaction for 1-2 hours, filter, and stir the sample in silica gel.After purification by column chromatography, the corresponding 5-trifluoromethyl-substituted 1,2,4-triazole compound (I) is obtained. The reaction process is shown by the following formula:

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, 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Zhejiang Sci-Tech University; Chen Zhengkai; Hu Sipei; Yang Zuguang; (10 pag.)CN110467579; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 32943-25-2, 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. 32943-25-2, name is 3-Chloro-10,11-dihydro-5H-dibenzo[b,f]azepine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 17 1-(3-(3-Chloro-10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)-1-propyl)4-piperidinecarboxylic acid hydrochloride 3-Chloro-10,11-dihydro-5H-dibenz[b,f]azepine (3.82 g, 16.6 mmol) was dissolved in toluene (20 ml). A solution of 3-chloropropionylchloride (2.53 g, 19.9 mmol) in toluene was added dropwise, and the resulting mixture was heated to 95 C. and stirred at that temperature for 30 minutes. The mixture was stirred overnight at room temperature. Further 3-chloropropionylchloride (2.53 g, 19.9 mmol) was added and the mixture was stirred at 95 C. for 1.5 h. After cooling, 0.2 M sodium hydroxide (10 ml) was added, and the phases were separated. The organic phase was diluted with more toluene (50 ml); and washed with first 0.2 M sodium hydroxide (6*10 ml) and then with more 0.2 M sodium hydroxide (3*20 ml) until the aqueous phase was alkaline. The organic phase was washed with water (3*15 ml), brine (25 ml), and dried (MgSO4). Evaporation in vacuo afforded 5.23 g (98%) of crude 3-chloro-1-(3-chloro-10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)-1-propanone as an oil. This was further purified by addition of a mixture of heptane and ethyl acetate (1:1). This afforded 3.14 g (59%) of the product as a solid.

The synthetic route of 3-Chloro-10,11-dihydro-5H-dibenzo[b,f]azepine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Novo Nordisk A/S; US6239148; (2001); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 7781-10-4, These common heterocyclic compound, 7781-10-4, name is 4-Chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidine, 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.

1.40 g (8 [MMOL)] of 3-methoxycarbonyl-1 H-indole are added to 30 cm3 of dimethylformamide at a temperature in the region of [20C] under an argon atmosphere, and 0.32 g (10 [MMOL)] of sodium hydride are then added. The reaction mixture is stirred at a temperature in the region of [20C] for 1 hour, 1.35 g (8.05 [MMOL)] of 4-chloro-7- methyl-7H-pyrrolo [2,3-d] pyrimidine in 10 cm3 of dimethylformamide are then added, and the mixture is heated at a temperature in the region of [100C] for 16 hours. The reaction mixture is then cooled to a temperature in the region of [20C] and then poured into a mixture of 200 cm3 of ethyl acetate and 200 cm3 of water. The organic phase is separated out after the phases have settled, washed with twice 200 cm3 of water and then with 200 cm3 of saturated aqueous sodium chloride solution, and then dried over magnesium sulphate and concentrated to dryness under reduced pressure (2.7 kPa). The residue is purified by flash chromatography on silica gel [eluent : cyclohexane/ethyl acetate (80/20 by volume)]. After the fractions containing the expected product have been concentrated to dryness under reduced pressure (2.7 kPa), 1.35 g of 3- [METHOXYCARBONYL-1- (7-METHYL-7H-PYRROLO] [2,3-d] pyrimidin-4-yl)-1 H-indole are obtained in the form of an off-white solid. Mass spectrum [(EL)] : m/e 306 [(M+)] (base peak).

The synthetic route of 7781-10-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AVENTIS PHARMA DEUTSCHLAND GMBH; WO2004/7479; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 461432-23-5, 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. 461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Take 32 kg of 5-bromo-2-chloro-4′-ethoxydiphenylmethane, add 100 kg (1:4) of anhydrous THF/toluene to the 500 liter reactor under nitrogen, and cool the liquid nitrogen to – 78 C,34 L of a 1.6 mol¡¤L-1 n-butyllithium hexane solution was slowly added dropwise, and the mixture was stirred at this temperature for 1 h. Will be cold to -78 C2,3,4,6-tetra-O-trimethylsilyl-D-gluconolactone100 kg of a toluene solution (26 kg) was slowly added dropwise to the above reaction liquid, and reacted at -78 C for 3 hours. After the completion of the reaction, 50 kg of a methanol solution of methanesulfonic acid (23 kg of methanesulfonic acid + 27 kg of methanol) was added thereto. The reaction was stirred at 0 C for 4 h, then warmed to 40 C and stirred for 7 h. A 5 mol¡¤L-1 aqueous sodium hydroxide solution was added to the reaction solution to adjust the pH to 7-8. After stirring for 30 min, it was extracted with ethyl acetate (50 kg¡Á2). The organic phase was washed with saturated aqueous sodium chloride to neutral, then dried over anhydrous sodium sulfateA yellowish viscous oil was obtained in an amount of 34.6 kg, yield 78%.

The synthetic route of 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Southeast University; Chen Junqing; Zhang Xiaolu; (9 pag.)CN108084130; (2019); B;,
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. 328-84-7, name is 3,4-Dichlorobenzotrifluoride, A new synthetic method of this compound is introduced below., Recommanded Product: 328-84-7

COMPARATIVE EXAMPLE 1 Synthesis of 2,3-dichloro-5-trifluoromethylbenzaldehyde STR13 57.3 g of 3,4-dichlorobenzotrifluoride was dissolved in 500 ml of dried tetrahydrofuran under nitrogen atmosphere and was cooled down to -78 C. To the resulting solution was dropped 200 ml of 1.6M hexane solution of n-butyl lithium. After the solution was further stirred for about 1.5 hours at the same temperature, 38.9 g of DMF was added dropwise into the reaction solution. After the completion of the addition, the temperature of the reaction system was gradually elevated to room temperature, while checking the progress of the reaction. Ice water was added to the reaction solution to extract with ether. The extract was dried over anhydrous magnesium sulfate. The solvent was distilled under reduced pressure. The obtained oily product was distilled under reduced pressure to give 45.3 g of oily residue (bp. 70~85 C./2 mmHg).

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; Nippon Soda Co., Ltd.; US5977414; (1999); 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. 108-70-3, name is 1,3,5-Trichlorobenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C6H3Cl3

Add phenothiazine,1,3,5-trichlorobenzene,Cuprous iodide,18-Crown-6 and potassium carbonate were added to the single-mouth round bottom flask.Sealed then protected by nitrogen,Add o-dichlorobenzene to dissolve and stir,The reaction was refluxed at 185C for 24 h.After the reaction was completed, the reaction solution was quenched by the addition of deionized water and then extracted with dichloromethane. The organic phase was dried over anhydrous sodium sulfate and concentrated under reduced pressure. Finally, a white solid product was obtained after purification by chromatography column in 31% yield.

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; Nanjing Tech University; An Zhongfu; Huang Wei; Wu Qi; Shi Huifang; (13 pag.)CN107793377; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 19230-27-4, name is 1,3-Dibromo-2-chlorobenzene, 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 19230-27-4, Recommanded Product: 1,3-Dibromo-2-chlorobenzene

To a mixture of 1,3-dibromo-2-chlorobenzene (Combi-Blocks catQA-2717: 2.2 g, 8.14 mmol), Pd(OAc)2 (0.183 g, 0.814 mmol) and cesium carbonate (6.63 g, 20.34 mmol) in 1,4-dioxane (30 ml) was added 1,4-dioxa-8-azaspiro[4.5]decane (Aldrich cat178365: 1.165 g, 8.14 mmol) under N2. The reaction mixture was stirred at 90 C. overnight. After the reaction was cooled to room temperature it was quenched with saturated aqueous NaHCO3, and extracted with ethyl acetate (3¡Á50 mL). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on a silica gel column with ethyl acetate in hexanes (0-20%) to afford the desired product. LC-MS calculated for C13H16BrClNO2 (M+H)+: m/z 332.0; found: 332.0/334.0.

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, 1,3-Dibromo-2-chlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Incyte Corporation; Wu, Liangxing; Qian, Ding-Quan; Lu, Liang; Lajkiewicz, Neil; Konkol, Leah C.; Li, Zhenwu; Zhang, Fenglei; Li, Jingwei; Wang, Haisheng; Xu, Meizhong; Xiao, Kaijiong; Yao, Wenqing; (101 pag.)US2018/177784; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics