HRID323510

反应详情

EQUATION

反应方程式

HRID 323510 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Combine (1-(2-(t-butyldimethylsilyloxy)ethyl)-1H-benzimidazol-2-yl)(1-(ethoxycarbonyl)piperidin-4-yl)amine (0.53 g, 12 mmol) and ammonium fluoride (2.667 g, 72 mmol) in methanol (60 mL). Heat to about 60° C. After 2.5 hours, cool, evaporate in vacuo and partition the evaporated reaction mixture between dichloromethane and a saturated aqueous sodium bicarbonate solution. Separate the layers and extract the organic layer twice with water and then brine. Dry the organic layer over MgSO4, filter, and evaporate in vacuo to give (1-(2-hydroxyethyl)-1H-benzimidazol-2-yl)(1-(ethoxycarbonyl)piperidin-4-yl)amine.

WORKUP

后处理

  1. temperaturecool
  2. customevaporate in vacuo
  3. custompartition
  4. customthe evaporated reaction mixture between dichloromethane
  5. customSeparate the layers
  6. extractionextract the organic layer twice with water
  7. dry with materialDry the organic layer over MgSO4
  8. filtrationfilter
  9. customevaporate in vacuo