반응식
[OH:1][CH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.I[CH:9]([CH2:11][CH2:12][CH2:13][CH3:14])[CH3:10]>CC(CC)=O>[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([CH2:10][CH2:9][CH2:11][CH2:12][CH2:13][CH3:14])[CH2:4][CH2:3]1참가 물질
4
실험 절차
4-Hydroxypiperidine (2.02 g, 20 mmol) was dissolved in 100 mL of methyl ethylketone. To this stirred mixture was added 2-iodohexane (1.5 mL, 10 mmol) and the resulting solution was heated at reflux for 1.5 hours. The mixture was allowed to cool and was then washed with saturated aqueous sodium bicarbonate (3×75 mL). The organic layer was dried over magnesium sulfate, filtered, and evaporated, and the residue was dried overnight under house vacuum to yield 1.184 g (64%) of the title compound which was used without further purification. 1H NMR consistent with desired product. MS(FD) 186(M+).
후처리
- temperaturethe resulting solution was heated
- temperatureat reflux for 1.5 hours
- temperatureto cool
- washwas then washed with saturated aqueous sodium bicarbonate (3×75 mL)
- dry with materialThe organic layer was dried over magnesium sulfate
- filtrationfiltered
- customevaporated
- customthe residue was dried overnight under house vacuum
출처 및 근거
- ORD 기록
- ord-e3f26c66634643b08fe45bb101c390a3
- 출처 데이터셋
- uspto-grants-2000_05
- 특허 번호
- US06060488
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