HRID280595

反应详情

EQUATION

反应方程式

HRID 280595 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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°.

WORKUP

后处理

  1. temperatureThe resulting solution was heated
  2. temperatureunder reflux for 2 hours
  3. temperaturecooled
  4. washwashed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated
  7. customThe residue was crystallised from methanol/water