Sulfuryl chloride → 3-Chloro-2-methylbenzo[b]thiophene-5-carboxylic acid methyl ester
反応式
S(Cl)([Cl:4])(=O)=O.[CH3:6][O:7][C:8]([C:10]1[CH:19]=[CH:18][C:13]2[S:14][C:15]([CH3:17])=[CH:16][C:12]=2[CH:11]=1)=[O:9]>C(Cl)(Cl)Cl>[CH3:6][O:7][C:8]([C:10]1[CH:19]=[CH:18][C:13]2[S:14][C:15]([CH3:17])=[C:16]([Cl:4])[C:12]=2[CH:11]=1)=[O:9]参加物
4
実験手順
Sulphuryl chloride (3.38 g) was added dropwise to a stirred solution of 2-methylbenzo[b]thiophene-5-carboxylic acid methyl ester (5.15 g) in chloroform (50 ml). The resulting solution was heated under reflux for 2 hours, cooled, washed with water, dried (Na2SO4) and evaporated. The residue was crystallised from methanol/water to give 3-chloro-2-methylbenzo[b]thiophene-5-carboxylic acid methyl ester, 3.00 g, m.p. 85°-86°.
後処理
- temperatureThe resulting solution was heated
- temperatureunder reflux for 2 hours
- temperaturecooled
- washwashed with water
- dry with materialdried (Na2SO4)
- customevaporated
- customThe residue was crystallised from methanol/water
出典と根拠
- ORDレコード
- ord-303769ecf52749dcbe676936c33968cf
- 出典データセット
- uspto-grants-1985_01
- 特許番号
- US04496572
反応ノート
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