HRID606457

反应详情

EQUATION

反应方程式

HRID 606457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of ethyl 3-[1-(triphenylmethyl)-1H-1,2,4-triazol-3-yl]propanoate obtained in Reference Example 24 (700 mg, 1.70 mmol) in THF (5 mL) was added to a suspension of lithium aluminum hydride (84.0 mg, 2.21 mmol) in THF (5 mL) at 0° C., and the mixture was stirred at 0° C. for 5 hr, and then at room temperature for 15 hr. Water and 1N aqueous sodium hydroxide solution were added to the mixture, and the insoluble material was filtered off. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (0-80% ethyl acetate/hexane) to give the title compound as a white powder (289 mg, 46%).

WORKUP

后处理

  1. waitat room temperature for 15 hr
  2. filtrationthe insoluble material was filtered off
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (0-80% ethyl acetate/hexane)