反応式
[CH3:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][CH:8]=2)[S:4][C:3]=1[CH:17]([OH:19])[CH3:18]>O=[Mn]=O>[CH3:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:8]=[CH:9][C:10]([C:13]([F:16])([F:14])[F:15])=[CH:11][CH:12]=2)[S:4][C:3]=1[C:17](=[O:19])[CH3:18]参加物
3
実験手順
To a solution of 1-[3-Methyl-5-(4-trifluoromethyl-phenyl)-thiophen-2-yl]-ethanol (see Preparation 2)(4.40 g, 15.4 mmole), is added MnO2 (7.88 g, 77.0 mmole) in one portion. The mixture is heated under reflux for 16 hours, more MnO2 (7.88 g, 77.0 mmole) is added to the reaction and continued to reflux for 4 hours. The mixture is filtered through a celite pad, and the mother liquid is concentrated. The crude product is purified on a silica gel column, gradient eluting with 0-20% ethyl acetate in hexane and concentrated to provide the titled compound as yellow solid.
後処理
- temperatureThe mixture is heated
- temperatureunder reflux for 16 hours
- temperatureto reflux for 4 hours
- filtrationThe mixture is filtered through a celite pad
- concentrationthe mother liquid is concentrated
- customThe crude product is purified on a silica gel column
- washgradient eluting with 0-20% ethyl acetate in hexane
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-617d2c25a5ed444db23b3ce802b6ae6c
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07504433B2
関連ノート
読み込み中…