Thionyl Chloride → 1-Chloro-4-(chloromethyl)-2,5-difluorobenzene
反応式
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([CH2:9]O)=[C:4]([F:11])[CH:3]=1.S(Cl)([Cl:14])=O>>[Cl:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH2:9][Cl:14])=[CH:6][C:7]=1[F:8]参加物
3
反応条件
- 温度
- 100 °C
実験手順
Step B A mixture of (4-chloro-2,5-difluoro-phenyl)-methanol (5.5 g, 32 mmol) in thionyl chloride (25 mL) was heated at refluxing (100° C.) for 30 min. The mixture was cooled to room temperature and concentrated. The residue was diluted with ethyl acetate, washed with saturated aqueous NaHCO3 solution, water, brine, dried over MgSO4, and concentrated to give 1-chloro-4-chloromethyl-2,5-difluoro-benzene as a yellow oil (2.1 g, 34%).
後処理
- temperaturewas heated
- temperatureThe mixture was cooled to room temperature
- concentrationconcentrated
- additionThe residue was diluted with ethyl acetate
- washwashed with saturated aqueous NaHCO3 solution, water, brine
- dry with materialdried over MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-1890021a17c8485abebe3a6404224499
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08354444B2
反応ノート
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