Chloroform → 3,5-Dichloro-2,6-dimethoxybenzoic Acid
反応式
S(Cl)([Cl:4])(=O)=O.[CH3:6][O:7][C:8]1C=[CH:15][CH:14]=[C:13]([O:17][CH3:18])[C:9]=1[C:10]([OH:12])=[O:11].[CH:19]([Cl:22])(Cl)Cl>>[Cl:4][C:14]1[C:13]([O:17][CH3:18])=[C:9]([C:8]([O:7][CH3:6])=[C:19]([Cl:22])[CH:15]=1)[C:10]([OH:12])=[O:11]参加物
4
実験手順
A solution of 20 ml (0.25 mol) of sulphuryl chloride in 50 ml of chloroform is added dropwise to a solution of 15.0 g (0.08 mol) 2,6-dimethoxybenzoic acid in 100 ml of chloroform. The solution is left over night at room temperature and is then refluxed for 0.5 h. The solvent is evaporated and the residue recrystallized twice from light petroleum. Yield: 17.0 g, m.p. 98°-100° C. (first recrystallization). Yield: 12.0 g, m.p. 102°-103° C. (second recrystallization).
後処理
- waitThe solution is left over night at room temperature
- temperatureis then refluxed for 0.5 h
- customThe solvent is evaporated
- customthe residue recrystallized twice from light petroleum
- customYield: 17.0 g, m.p. 98°-100° C. (first recrystallization)
- customYield: 12.0 g, m.p. 102°-103° C. (second recrystallization)
出典と根拠
- ORDレコード
- ord-d793655f80324e32b5c6fdf764de3020
- 出典データセット
- uspto-grants-1980_11
- 特許番号
- US04232037
反応ノート
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