HRID389935

反应详情

EQUATION

反应方程式

HRID 389935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

N-methylpiperazine (25.4 mmol) was added to a suspension of ethyl 5-(2,4-bis(benzyloxy)-5-chlorophenyl)isoxazole-3-carboxylate (2.1 mmol) in EtOH (5 ml) and the reaction mixture was heated to 90° C. under stirring for 18 h. The reaction mixture was poured into a mixture of water (15 ml) and AcOEt (30 ml). After standard extraction, the organic layer was washed with water and brine, dried over Na2SO4, and evaporated. The resulting solid was purified by silica gel column chromatography (CHCl3/MeOH: 95/0.5) to give the desired compound (620 mg, 57%).

WORKUP

后处理

  1. extractionAfter standard extraction
  2. washthe organic layer was washed with water and brine
  3. dry with materialdried over Na2SO4
  4. customevaporated
  5. customThe resulting solid was purified by silica gel column chromatography (CHCl3/MeOH: 95/0.5)