Thionyl Chloride → HCID 22648742、化合物
反応式
O[CH:2]([C:6]1[C:7]([C:12]([F:15])([F:14])[F:13])=[N:8][CH:9]=[N:10][CH:11]=1)[CH:3]([CH3:5])[CH3:4].S(Cl)([Cl:18])=O>C(Cl)(Cl)Cl>[Cl:18][CH:2]([C:6]1[C:7]([C:12]([F:15])([F:14])[F:13])=[N:8][CH:9]=[N:10][CH:11]=1)[CH:3]([CH3:5])[CH3:4]参加物
4
実験手順
22 g (100 mmol) of 5-(1-hydroxy-2-methylpropyl)-4-trifluoromethylpyrimidine was dissolved in 150 ml of chloroform, and 25 ml (342 mmol) of thionyl chloride was added. The reaction mixture was heated and refluxed for 2 hours. The solvent and thionyl chloride was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (developing solvent/n-hexane:ethyl acetate=6:1) to obtain 11.6 g (yield: 49%) of 5-(1-chloro-2-methylpropyl)-4-trifluoromethylpyrimidine as brown liquid (refractive index nD20: 1.4558).
後処理
- temperatureThe reaction mixture was heated
- temperaturerefluxed for 2 hours
- distillationThe solvent and thionyl chloride was distilled off under reduced pressure
- customthe residue was purified by silica gel column chromatography (developing solvent/n-hexane:ethyl acetate=6:1)
出典と根拠
- ORDレコード
- ord-382c8f248abf4678904bdb1da588f576
- 出典データセット
- uspto-grants-2004_10
- 特許番号
- US06806230B1
反応ノート
読み込み中…