HRID1862493

反应详情

EQUATION

反应方程式

HRID 1862493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (S)-N-[2-(4-hydroxy-3-methoxy-phenyl)-ethyl]-2-methanesulfonylamino-3-methyl-butyramide (2.5 g), E-(3-bromo-propenyl)-benzene(1.5 g) and sodium methoxide (9 ml 1M solution in methanol) in methanol (30 ml) is heated to reflux for 4 hours. Upon cooling water (400 ml) is added. The mixture is extracted with ethyl acetate (2×300 ml). The organic layers are washed with brine (100 ml), dried (MgSO4) and evaporated. The resulting residue is purified by recrystallisation (ethyl acetate/hexane). E-(S)-2-Ethanesulfonylamino-N-{2-[3-methoxy-4-(3-phenyl-allyloxy)-phenyl]-ethyl}-3-methyl-butyramide is obtained, m.p. 128-133° C.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureto reflux for 4 hours
  3. additionis added
  4. extractionThe mixture is extracted with ethyl acetate (2×300 ml)
  5. washThe organic layers are washed with brine (100 ml)
  6. dry with materialdried (MgSO4)
  7. customevaporated
  8. customThe resulting residue is purified by recrystallisation (ethyl acetate/hexane)