HRID1906936

反应详情

EQUATION

反应方程式

HRID 1906936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of toluene (100 ml), 50% sodium hydroxide (20 ml), 3-phenylsulfinylindole (4.27 g, 17.7 mmol) and benzyltrimethylammonium chloride (6.01 g, 26.5 mmol) was vigorously stirred at reflux temperature for 4 hours. The organic phase was separated and combined with an ether extract of the aqueous phase. The extract was dried and evaporated in vacuo giving a solid which on crystallization from dichloromethane-hexane gave the solid product. Chromatography of the mother liquor on silica gel using hexane-ethyl acetate (3:2) as the eluant gave a further quantity of the title compound, m.p. 148°-149° C. identical to the material prepared in Example 8.

WORKUP

后处理

  1. temperatureat reflux temperature for 4 hours
  2. customThe organic phase was separated
  3. extractionextract of the aqueous phase
  4. customThe extract was dried
  5. customevaporated in vacuo
  6. customgiving a solid which
  7. customon crystallization from dichloromethane-hexane
  8. customgave the solid product