2-CHLORO-N-(2-METHYLPHENYL)PROPANAMIDE synthesis
- Product Name:2-CHLORO-N-(2-METHYLPHENYL)PROPANAMIDE
- CAS Number:19281-31-3
- Molecular formula:C10H12ClNO
- Molecular Weight:197.66
Yield:19281-31-3 95%
Reaction Conditions:
Stage #1:(R,S)-2-chloropropionic acid with 2-chloro-4,6-dimethoxy-1 ,3,5-triazine in N,N-dimethyl-formamide for 0.25 h;
Stage #2:o-toluidine with 4-methyl-morpholine in water;N,N-dimethyl-formamide at 0 - 10; for 6.25 h;
Steps:
1 Preparation of cocaine base intermediate (type ) propylamine Example 1
2-Chloro-4,6-dimethoxy-1,3,5-triazine 35.11g (0.2mol) was added to 400mlN, N- dimethylformamide was stirred to dissolve and cooled to 0 deg.] C, was added 2-chloro- propionic acid (formula ) 21.70g (0.2mol), stirring was continued for 15min, a solution of o-toluidine (formula ) 21.43g (0.2mol) was added dropwise slowly and evenly stirred 15min N- methylmorpholine 20.23g (0.2mol) drops for 4 hours to complete insulation.Stirring dropping water 1L, completion of control at 0-10 drop crystallization 2h.Crystalline suction filtered to dryness, the filter cake at atmospheric pressure 60 dried to give a white solid N- (2- methylphenyl) -2-chloropropionyl amide (Formula ) 37.71g, molar yield 95%.
References:
Chongqing Leisure Pharmaceutical Co., Ltd;Chen, Wenhui;Yang, Zhongxin;Ge, Xiaoqiang;Zhang, Yusheng;Zou, Yulong;Zhang, Qiang;Yang, Jibin;Cai, Zhongwen CN105439887, 2016, A Location in patent:Paragraph 0016
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