Chloroform → 3,5-Dichloro-2,6-dimethoxybenzoic Acid
반응식
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]참가 물질
4
실험 절차
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).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-d793655f80324e32b5c6fdf764de3020
- 출처 데이터셋
- uspto-grants-1980_11
- 특허 번호
- US04232037
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