Ammonium Hydroxide → 3-(4-Methoxycyclohexyl)-pyrrolidin-2-one
반응식
[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][CH:6]([CH:9]2[CH2:13][CH2:12][O:11][C:10]2=O)[CH2:5][CH2:4]1.[OH-].[NH4+:16]>C(O)C>[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][CH:6]([CH:9]2[CH2:13][CH2:12][NH:16][C:10]2=[O:11])[CH2:5][CH2:4]1참가 물질
4
실험 절차
Heat a mixture of 3-(4-methoxycyclohexyl)-dihydro-furan-2-one (0.91 g), ammonium hydroxide (20 mL) and ethanol (20 mL) at 230° C. in a sealed steel bottle for 12 hours. Cool the reaction and remove the solvent in vacuo. Partition the residue with ethyl acetate (100 mL) and HCl (1N, 60 mL). Dry the organic over sodium sulfate. After filtration and concentration, recrystallize with 1:3 ethyl acetate:hexane to afford 0.71 gram of the title compound.
후처리
- temperatureHeat
- temperatureCool
- customthe reaction
- customremove the solvent in vacuo
- customPartition the residue with ethyl acetate (100 mL) and HCl (1N, 60 mL)
- dry with materialDry the organic over sodium sulfate
- filtrationAfter filtration and concentration
- customrecrystallize with 1:3 ethyl acetate
출처 및 근거
- ORD 기록
- ord-59ef374852b84706b8aaff523165ce83
- 출처 데이터셋
- uspto-grants-2011_08
- 특허 번호
- US07994176B2
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