2-ThiophenecarboxaMide, 5-chloro-N-Methyl- synthesis
- Product Name:2-ThiophenecarboxaMide, 5-chloro-N-Methyl-
- CAS Number:97799-98-9
- Molecular formula:C6H6ClNOS
- Molecular Weight:175.64
Yield: 49.24%
Reaction Conditions:
Stage #1:5-Chlorothiophene-2-carboxylic acid with thionyl chloride in dichloromethane at 0 - 20; for 6 h;
Stage #2:methylamine in dichloromethane;water at 0 - 20; for 16 h;
Steps:
10.1-10.3; 11.1-11.3; 12.1-12.3
Step Add 5-chlorothiophene-2-carboxylic acid and dichloromethane to the reaction vessel D, and add dichlorosulfoxide dropwise at 0 ° C. After the dropwise addition, stir at room temperature for 6 hours;After step , an aqueous solution of 40% methylamine was added dropwise at 0 ° C, and the dropwise addition was completed, followed by stirring at room temperature for 16 hours;After step , suction filtration was performed, and the cake was dried at 50 ° C to constant weight, and the solid was the impurity D.5-chlorothiophene-2-carboxylic acid, dichloromethane, dichlorosulfoxide, 40% methylamine in water were added in an amount of 20 g, 500 ml, 49.52 g, 107.73 g;The reaction vessel D is a 1L four-necked bottle;The impurity D was 12 g, the yield was 49.24%, and the purity was 99.71%.
References:
Xinxiang Shuanglu Pharmaceutical Co., Ltd.;Li Pu;Lv Zhenpei;Guo Benquan CN110357868, 2019, A Location in patent:Paragraph 0166-0194
![Ethanamine, N-[(3,5-dichlorophenyl)methylene]-2,2-diethoxy-](/CAS/20210305/GIF/1000210-73-0.gif)
1000210-73-0
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