Nitromethane → Ethyl 5-methyl-3-nitromethylheptanoate
反応式
[CH3:1][CH:2]([CH2:11][CH3:12])[CH2:3][CH:4]=[CH:5][C:6]([O:8][CH2:9][CH3:10])=[O:7].C1CCN2C(=NCCC2)CC1.[N+:24]([CH3:27])([O-:26])=[O:25]>C(#N)C>[CH3:1][CH:2]([CH2:11][CH3:12])[CH2:3][CH:4]([CH2:27][N+:24]([O-:26])=[O:25])[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7]参加物
5
実験手順
Ethyl 5-methyl-2-heptanoate 12 (6.75 g, 39.70 mmol), DBU (6.0 g, 39.7 mmol), nitromethane (21.97 g, 359.9 mmol) in acetonitrile 80 mL was stirred at room temperature under nitrogen atmosphere overnight. The mixture was concentrated to an oil. A solution of the oil in ether was washed with 1N HCl, brine and dried. It was evaporated to give a light oil which was chromatographed on silica gel, eluting with 5% to 10% ether in Pet. ether to give 13 (3.6 g, 42%).
後処理
- concentrationThe mixture was concentrated to an oil
- washA solution of the oil in ether was washed with 1N HCl, brine
- customdried
- customIt was evaporated
- customto give a light oil which
- customwas chromatographed on silica gel
- washeluting with 5% to 10% ether in Pet. ether
出典と根拠
- ORDレコード
- ord-68281862548f4864a49ad3dd305d88eb
- 出典データセット
- uspto-grants-2006_04
- 特許番号
- US07026505B2
反応ノート
読み込み中…