HRID606452

反应详情

EQUATION

反应方程式

HRID 606452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-[(2-{[1-(triphenylmethyl)-1H-1,2,4-triazol-3-yl]thio}ethyl)oxy]pyridine-4-carbonitrile obtained in Reference Example 19 (5.00 g, 10.2 mmol) in THF (40 mL) was added to a suspension of lithium aluminum hydride (0.775 g, 20.4 mmol) in THF (60 mL) at 0° C., and the mixture was stirred at room temperature for 7 hr. The mixture was cooled to 0° C., water and 1N aqueous sodium hydroxide solution were added, and the insoluble material was filtered off. The filtrate was dried over sodium sulfate, and concentrated. The obtained oil was purified by silica gel column chromatography (0-20% methanol/ethyl acetate) to give the title compound as a yellow oil (2.06 g, 41%).

WORKUP

后处理

  1. temperatureThe mixture was cooled to 0° C.
  2. filtrationthe insoluble material was filtered off
  3. dry with materialThe filtrate was dried over sodium sulfate
  4. concentrationconcentrated
  5. customThe obtained oil was purified by silica gel column chromatography (0-20% methanol/ethyl acetate)