반응식
[C:1]([O:9]CC)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.[CH2:12]([S:19][CH2:20][CH2:21][NH2:22])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.CC>>[CH2:12]([S:19][CH2:20][CH2:21][NH:22][C:1](=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1참가 물질
4
실험 절차
30 grams of ethyl nicotinate and 80 grams of 2-benzylthio ethylamine are heated for 12 hours at 170°-180° C. The ethane liberated during the reaction is removed by means of a Dean Stark apparatus. After cooling, the reaction mixture is dissolved in 400 cc of carbon tetrachloride; by addition of petroleum ether, the N-(2-benzylthioethyl)nicotinamide crystallizes: 47 g. By crystallization in a mixture of carbon tetrachloride and cyclohexane, there are recovered colorless crystals of the above product melting at 79° C.
후처리
- customis removed by means of a Dean Stark apparatus
- temperatureAfter cooling
- dissolutionthe reaction mixture is dissolved in 400 cc of carbon tetrachloride
- additionby addition of petroleum ether
- customthe N-(2-benzylthioethyl)nicotinamide crystallizes
- customBy crystallization
- additionin a mixture of carbon tetrachloride and cyclohexane, there
- customare recovered colorless crystals of the above product melting at 79° C.
출처 및 근거
- ORD 기록
- ord-364575368ff64c4f82e9fa07664cbb26
- 출처 데이터셋
- uspto-grants-1980_05
- 특허 번호
- US04204064
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