HRID1979533

反应详情

EQUATION

反应方程式

HRID 1979533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-50 °C

PROCEDURE

实验过程

The reaction mixture is stirred at -50° C. for 20 minutes, a solution of 2.75 g (0.0125 mol) of the nitrile prepared under (a) in 10 cc of THF is then added dropwise, the mixture is stirred again at -50° C. for 30 minutes and a solution of 3 g of the compound prepared under (b) in 10 cc of THF is then added. The reaction mixture is stirred for 1 hour at -50° C. and then left to stand overnight at ambient temperature. It is poured into 0.5 liter of a water/ice mixture, saturated with NaCl and extracted with diethyl ether. The organic phase is dried and evaporated. The oil obtained is chromatographed on a silica 60 column, elution being carried out with a 70/30 CH2Cl2 /acetone mixture.

WORKUP

后处理

  1. additionis then added dropwise
  2. stirringthe mixture is stirred again at -50° C. for 30 minutes
  3. additionis then added
  4. stirringThe reaction mixture is stirred for 1 hour at -50° C.
  5. waitleft
  6. waitto stand overnight at ambient temperature
  7. extractionextracted with diethyl ether
  8. customThe organic phase is dried
  9. customevaporated
  10. customThe oil obtained
  11. customis chromatographed on a silica 60 column, elution