Thionyl Chloride → 5-Chloro-2-methoxybenzoyl chloride
反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][C:4]=1[C:5](O)=[O:6].O=S(Cl)[Cl:15]>>[Cl:12][C:9]1[CH:10]=[CH:11][C:3]([O:2][CH3:1])=[C:4]([CH:8]=1)[C:5]([Cl:15])=[O:6]参加物
3
実験手順
A solution of 2-methoxy-5-chlorobenzoic acid (0.37 g, 2.0 mmol) in 10 mL of SOCl2 was warmed to reflux and was allowed to stir for 2 hours. The mixture was cooled to ambient temperature and concentrated under reduced pressure. The crude material was diluted with 5 mL of toluene and concentrated under reduced pressure. This dilution with toluene and concentration was repeated two additional times to afford the title compound. 1H NMR (300 MHz, dimethylsulfoxide-d6) δ ppm 3.82 (s, 3H), 7.16 (d, J=8.8 Hz, 1H), 7.49-7.59 (m, 1H), 7.61 (d, J=2.7 Hz, 1H).
後処理
- temperatureto reflux
- concentrationconcentrated under reduced pressure
- additionThe crude material was diluted with 5 mL of toluene
- concentrationconcentrated under reduced pressure
- concentrationThis dilution with toluene and concentration
出典と根拠
- ORDレコード
- ord-4145f52b9e1d4a9998d5b6cbd54e621c
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841334B2
反応ノート
読み込み中…