HRID1368100

反应详情

EQUATION

反应方程式

HRID 1368100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-[4-[2-[4-methyl-2-propyl-6-oxo-1,6-dihydro-1-pyrimidinyl]ethoxy]phenyl methylene]thiazolidine-2,4-dione (5.0 g, 12.46 mmol) obtained from example 1 in 1,4-dioxane (75 ml) was reduced with hydrogen in the presence of 10% palladium on charcoal (12.0 g) at 60 psi pressure for 40 h. The mixture was filtered through a bed of celite. The fltrate was evaporated to dryness under reduced pressure, purified by cohun chromatography (2: 1 EtOAc/petroleum ether as eluent) followed by crystallization (CH2Cl2) to afford the title compound (4.6 g, 92%), mp 144-146° C.

WORKUP

后处理

  1. filtrationThe mixture was filtered through a bed of celite
  2. customThe fltrate was evaporated to dryness under reduced pressure
  3. custompurified by cohun chromatography (2: 1 EtOAc/petroleum ether as eluent)
  4. customfollowed by crystallization (CH2Cl2)