반응식
[CH3:1][N:2]1[CH2:12][CH2:11][CH2:10][CH2:9][CH:3]1[C:4]([O:6][CH2:7][CH3:8])=[O:5].[CH3:13][N:14](C)[CH2:15]CO.C([Sn](=O)CCCC)CCC>>[CH3:1][N:2]1[CH2:12][CH2:11][CH2:10][CH2:9][CH:3]1[C:4]([O:6][CH2:7][CH2:8][N:14]([CH3:15])[CH3:13])=[O:5]참가 물질
4
반응 조건
- 온도
- 145 °C
실험 절차
A mixture of 85 g (0.5 mol) of ethyl 1-methylpipecolinate, 44.6 g (0.5 mol) of N,N-dimethylethanolamine and 0.82 g of dibutyltin oxide was heated at about 145° C. for 30 hours. The ethanol by-product was collected in a Dean-Stark trap. When the rate of ethanol evolution and amount of ethanol collected showed that the reaction was essentially complete, the reaction was heated at about 180° C. until ethanol evolution ceased. The liquid product was purified by distillation at reduced pressure to provide 2-(N,N-dimethylamino)ethyl N-methylpipecolinate.
후처리
- customThe ethanol by-product was collected in a Dean-Stark trap
- customWhen the rate of ethanol evolution and amount of ethanol collected
- temperaturethe reaction was heated at about 180° C. until ethanol evolution
- distillationThe liquid product was purified by distillation at reduced pressure
출처 및 근거
- ORD 기록
- ord-6e74ee1cb88d4903a3fa856dd9a5d693
- 출처 데이터셋
- uspto-grants-1993_07
- 특허 번호
- US05225513
연결된 노트
불러오는 중…