Ammonium Hydroxide → 3-(4-Methoxycyclohexyl)-pyrrolidin-2-one
反応式
[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]1参加物
4
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-59ef374852b84706b8aaff523165ce83
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07994176B2
反応ノート
読み込み中…