反応式
[CH3:1][O:2][C:3]([CH2:5][CH:6]1[CH2:10][CH2:9][CH:8]([OH:11])[CH:7]1[CH2:12]/[CH:13]=[CH:14]\[CH2:15][CH3:16])=[O:4]>C(Cl)Cl>[CH3:1][O:2][C:3]([CH2:5][CH:6]1[CH2:10][CH2:9][C:8](=[O:11])[CH:7]1[CH2:12]/[CH:13]=[CH:14]\[CH2:15][CH3:16])=[O:4]参加物
3
反応条件
- 温度
- 18 °C
実験手順
A 150 mg quantity of 3-methoxycarbonylmethyl-2-(cis-2-pentenyl)-cyclopentanol is dissolved in 10 ml of methylene chloride. A 2 ml quantity of chromic acid solution of 2 M concentration is added dropwise to the solution. The mixture is stirred at about 18° C. for 12 hours and thereafter extracted with ethyl acetate. The extract is washed with aqueous solution of sodium chloride, dried and concentrated. The residue is purified with a silica gel column and distilled in a vacuum, affording 3-methoxycarbonylmethyl-2-(cis-2-pentenyl)-cyclopentanone (compound (4), R2 =CH3) in a yield of 88%, b.p. 92°-96° C./2.7 mm Hg.
後処理
- concentrationA 2 ml quantity of chromic acid solution of 2 M concentration
- additionis added dropwise to the solution
- extractionextracted with ethyl acetate
- washThe extract is washed with aqueous solution of sodium chloride
- customdried
- concentrationconcentrated
- customThe residue is purified with a silica gel column
- distillationdistilled in a vacuum
出典と根拠
- ORDレコード
- ord-067fa63bb80d4e94acebb1b91ba3278b
- 出典データセット
- uspto-grants-1980_12
- 特許番号
- US04237308
関連ノート
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