HRID2251981

反应详情

EQUATION

反应方程式

HRID 2251981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

Dissolve [1-(3,5-bis-trifluoromethyl-benzyl)-5-morpholin-4-yl-1H-[1,2,3]triazol-4-yl]-morpholin-4-yl-methanone in THF. Cool to −78° C., slowly add 28.3 ml (4 eq) of 1M diisobutyl aluminum hydride in toluene, and stir 2.5 hours. Move to 0° C. ice bath and allow reaction to slowly warm while stirring overnight. Slowly quench by adding ˜5 ml 1N HCl while still at 0° C. then warming to RT. Pour into 50 ml 1N NaOH. Extract with EtOAc, then wash organic layer with 1N HCl. Concentrate organic layer to give the desired aldehyde, which can be used without further purification. MS (IS) 409.2 (M+1). Rf=0.61 (1:1 Hexanes:EtOAc)

WORKUP

后处理

  1. customMove to 0° C.
  2. customreaction
  3. temperatureto slowly warm
  4. customSlowly quench
  5. additionby adding ˜5 ml 1N HCl while still at 0° C.
  6. temperaturethen warming to RT
  7. additionPour into 50 ml 1N NaOH
  8. extractionExtract with EtOAc