HRID402374

反应详情

EQUATION

反应方程式

HRID 402374 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

To a solution of 5-pyridin-2-yl-3-trimethylsilanylmethyl-3H-[1,2,3]triazole-4-carboxylic acid ethyl ester (1.67 g, 5.49 mmol) in dry THF (17 mL) was added portionwise lithiumaluminiumhydride (0.24 g, 6.31 mmol) at 0° C. and the reaction mixture was stirred at 0° C. for 1 h. Then water (240 μL) and NaOH (15%, 240 μL) was added followed by water (720 μL). The precipitate was then filtered off and the filtrate evaporated. Purification by chromatography (silica, 0 to 10% methanol in dichloromethane) afforded the title compound (379 mg, 26%) as a white solid. MS: m/e=263.1 [M+H]+.

WORKUP

后处理

  1. filtrationThe precipitate was then filtered off
  2. customthe filtrate evaporated
  3. customPurification by chromatography (silica, 0 to 10% methanol in dichloromethane)