Chloroform → 3,5-Dichloro-2,6-dimethoxybenzoic Acid

HRID 224418

반응식

HRID 224418 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

반응물 3

HCID 6212Chloroform2회HCID 151092,6-Dimethoxybenzoic AcidHCID 24648Sulfuryl chloride

생성물 1

HCID 27747503,5-Dichloro-2,6-dimethoxybenzoic Acid

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

  1. waitThe solution is left over night at room temperature
  2. temperatureis then refluxed for 0.5 h
  3. customThe solvent is evaporated
  4. customthe residue recrystallized twice from light petroleum
  5. customYield: 17.0 g, m.p. 98°-100° C. (first recrystallization)
  6. 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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