Thionyl Chloride → 1-(Chloromethyl)-4-fluoro-2-methylbenzene
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8]O)=[C:4]([CH3:10])[CH:3]=1.O=S(Cl)[Cl:13]>C(Cl)Cl>[Cl:13][CH2:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][C:4]=1[CH3:10]参加物
4
反応条件
- 温度
- 0 °C
実験手順
(4-Fluoro-2-methylphenyl)methanol (11.5 g, 82 mmol) was dissolved in CH2Cl2 (100 mL). The mixture was cooled to 0° C. before adding SOCl2 (10.7 g, 90 mmol), then stirred for 30 min at 0° C. and then at room temperature for 1.5 h. The solvent and excess of SOCl2 were removed by evaporation followed by the addition of CH2Cl2. The solvent and remaining traces of SOCl2 were evaporated once more. There was obtained 13.0 g (100%) of 1-(chloromethyl)-4-fluoro-2-methylbenzene as an oil. 1H NMR (300 MHz, CDCl3): 2.4 (s, 3H), 4.6 (s, 2H), 6.8-7.0 (m, 2H), 7.3 (m, 1H).
後処理
- waitat room temperature for 1.5 h
- customThe solvent and excess of SOCl2 were removed by evaporation
- additionfollowed by the addition of CH2Cl2
- customwere evaporated once more
出典と根拠
- ORDレコード
- ord-e4780ea8b04548c3aacbdfe22a6d5b38
- 出典データセット
- uspto-grants-2008_07
- 特許番号
- US07402581B2
反応ノート
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