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

HRID 224418

反応式

HRID 224418 の反応式
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

反応物 3

HCID 6212Chloroform2 回HCID 151092,6-Dimethoxybenzoic AcidHCID 24648Sulfuryl chloride

生成物 1

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

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

  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)

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

関連ノート

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