HRID1386075

反应详情

EQUATION

反应方程式

HRID 1386075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of LiAlH4 (0.08 g, 2.1 mmol) in tetrahydrofuran (15 ml) was added 3-carboethoxy-2,6-dimethyl-8-(2-ethyl-4-fluoro-6-methylbenzylamino)imidazo[1,2-a]pyridine (0.4g, 1.0) mmol in tetrahydrofuran (15 ml). After stirring the mixture at room temperature for 4 h., 0.1 ml of water was added dropwise, followed by 0.1 ml of 15% sodium hydroxide and then 0.3 ml of water. The solids were removed by filtration and washed thoroughly with tetrahydrofuran. The filtrate and washings were combined and dried and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel using methylene chloride:methanol (9:1) as eluent. Crystallization from acetonitril gave 0.32 g (89%) of the title compound.

WORKUP

后处理

  1. customThe solids were removed by filtration
  2. washwashed thoroughly with tetrahydrofuran
  3. customdried
  4. customthe solvent was removed under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel
  6. customCrystallization from acetonitril