HRID748056

反应详情

EQUATION

反应方程式

HRID 748056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a stirred solution of 1-(4-fluorobenzyl)-1H-1,2,4-triazole (0.500 g, 2.82 mmol) in THF (30 mL) at −78° C. was added a solution of n-butyllithium (2.5M in hexanes, 1.1 mL, 2.9 mmol) dropwise. The mixture was stirred at −78° C. for 1.5 h, then 2-ethylbutyraldehyde (0.42 mL, 3.4 mmol) was added. The solution was slowly warmed to room temperature and stirred i 8 h. It was then quenched with saturated aqueous NH4Cl and extracted twice with EtOAc. The organic extracts were dried (MgSO4), filtered, concentrated in vacuo and purified by column chromatography (SiO2, EtOAc/hexane, 1:1) to yield an oil in 47% yield.

WORKUP

后处理

  1. temperatureThe solution was slowly warmed to room temperature
  2. stirringstirred i 8 h
  3. customIt was then quenched with saturated aqueous NH4Cl
  4. extractionextracted twice with EtOAc
  5. dry with materialThe organic extracts were dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. custompurified by column chromatography (SiO2, EtOAc/hexane, 1:1)
  9. customto yield an oil in 47% yield