HRID2198603

反应详情

EQUATION

反应方程式

HRID 2198603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 7.6 g. portion of 4-(2-diisopropylaminoethoxy)benzoic acid, hydrochloride, was converted to the acid chloride as described in Example 1 above, and was used to acylate 5 g. of 6-methanesulfonyloxy-2-(4-methanesulfonyloxyphenyl)benzo[b]thiophene in the presence of 20 g. of aluminum chloride. Work up according to Example 4 gave 7.4 g. of crystalline product after trituration of the isolated oil with denatured ethanol. The product was recrystallized from denatured ethanol to obtain 6.5 g. of purified product, and a 1.5 g. portion was further purified by chromatography over silica gel, eluting with 1:3 methanol:chloroform to obtain 1.15 g. of analytical sample, m.p. 198°-201°.

WORKUP

后处理

  1. customgave 7.4 g
  2. customThe product was recrystallized from denatured ethanol
  3. customto obtain 6.5 g
  4. customportion was further purified by chromatography over silica gel
  5. washeluting with 1:3 methanol
  6. customchloroform to obtain 1.15 g