Thionyl Chloride → HCID 14770843、化合物
反応式
[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([CH:9]2[CH2:13][CH2:12][CH:11](O)[CH2:10]2)=[C:4]([F:15])[CH:3]=1.S(Cl)([Cl:18])=O>>[Br:1][C:2]1[CH:3]=[C:4]([F:15])[C:5]([CH:9]2[CH2:13][CH2:12][CH:11]([Cl:18])[CH2:10]2)=[CH:6][C:7]=1[F:8]参加物
3
実験手順
A solution of 27.7 g (0.1 mol) of 3-(4-bromo-2,5-difluorophenyl)cyclopentanol in 150 ml of thionyl chloride was heated at reflux until gas evolution ceased (4 hours). The solvent was removed in vacuo and the residue was triturated with toluene (2×200 ml) which was also removed in vacuo. The residue was dissolved in ether, washed with water (3×100 ml), dried (MgSO4), filtered, and evaporated in vacuo to give 26.2 g of the title compound which was used without further purification.
後処理
- temperatureat reflux until gas evolution
- custom(4 hours)
- customThe solvent was removed in vacuo
- customthe residue was triturated with toluene (2×200 ml) which
- customwas also removed in vacuo
- dissolutionThe residue was dissolved in ether
- washwashed with water (3×100 ml)
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-1bfc5690bf94406dba3109908e95ddcf
- 出典データセット
- uspto-grants-1990_05
- 特許番号
- US04929613
反応ノート
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