反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[O:10][C:11]([F:14])([F:13])[F:12])[CH2:5]Br.NC(N)=[S:17]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:5][SH:17])[CH:7]=[CH:8][C:9]=1[O:10][C:11]([F:14])([F:13])[F:12]参加物
4
実験手順
To a solution of 3-chloro-4-(trifluoromethoxy)benzylbromide (5 g) in ethanol (100 ml) was added thiourea (5 g) and the mixture heated under reflux for 2 hours. The mixture was evaporated to dryness and the residue taken up into water (100 ml). To this solution was added sodium hydroxide pellets (3 g) and the mixture heated under reflux for 1 hour. The mixture was allowed to cool to room temperature and acidified with concentrated hydrochloric acid, the mixture was extracted with ether, dried and evaporated to give the subtitle compound as a colourless waxy solid (3.5 g).
後処理
- temperaturethe mixture heated
- temperatureunder reflux for 2 hours
- customThe mixture was evaporated to dryness
- additionTo this solution was added sodium hydroxide pellets (3 g)
- temperaturethe mixture heated
- temperatureunder reflux for 1 hour
- extractionthe mixture was extracted with ether
- customdried
- customevaporated
出典と根拠
- ORDレコード
- ord-bcf0365a16f44fd1ad39f5ee8d7eebb8
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08143261B2
関連ノート
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