HRID1696733

反应详情

EQUATION

反应方程式

HRID 1696733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.40 g (55 mM) 5-(2-methoxy-ethyl)-4-methyl-thiophene-2-sulfonyl chloride in 20 ml acetone was added 5 ml of an aqueous solution of ammonia (25%) and the mixture was stirred at room temperature for 1 h. The mixture was partitioned between water and ethyl acetate. The phases were separated and the organic phase was dried over sodium sulfate and evaporated. The residue purified by chromatography on silica gel crystallized form cyclohexane/diethyl ether to yield 0.89 g of the title compound as light red solid. MS (ISN) M−H+=233.8

WORKUP

后处理

  1. customThe mixture was partitioned between water and ethyl acetate
  2. customThe phases were separated
  3. dry with materialthe organic phase was dried over sodium sulfate
  4. customevaporated
  5. customThe residue purified by chromatography on silica gel
  6. customcrystallized
  7. customform cyclohexane/diethyl ether