HRID606452
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was cooled to 0° C.
- filtrationthe insoluble material was filtered off
- dry with materialThe filtrate was dried over sodium sulfate
- concentrationconcentrated
- customThe obtained oil was purified by silica gel column chromatography (0-20% methanol/ethyl acetate)