Acetic Acid → HCID 19804848、化合物
反応式
[CH2:1]([O:8][CH:9]1[CH2:14][CH2:13]C(C#N)[CH2:11][CH2:10]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[C:18]([OH:21])(=[O:20])[CH3:19]>>[CH2:1]([O:8][CH:9]1[CH2:14][CH2:13][CH:19]([C:18]([OH:21])=[O:20])[CH2:11][CH2:10]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
The crude 4-benzyloxycyclohexane-1-nitrile (4.0 g) was refluxed with stirring with a mixture of glacial acetic acid (16 ml) and concentrated hydrochloric acid (24 ml) for 20 hours. The reaction mixture was cooled, the solid removed by filtration and washed with water. The product was ground with 2M sodium hydroxide solution (70 ml) and then diluted with water. Unchanged nitrile was removed by filtration and the filtrate acidified with concentrated hydrochloric acid. White crystals separated and were collected by filtration, washed with water and dried to yield 4-benzyloxycyclohexane-1-carboxylic acid m.p. 170°-180° C.
後処理
- temperatureThe reaction mixture was cooled
- customthe solid removed by filtration
- washwashed with water
- additiondiluted with water
- customUnchanged nitrile was removed by filtration
- customWhite crystals separated
- filtrationwere collected by filtration
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-3aa3c5219a44421d8de6d73e59c11f0a
- 出典データセット
- uspto-grants-1991_10
- 特許番号
- US05053432
反応ノート
読み込み中…