HRID1981194

反应详情

EQUATION

反应方程式

HRID 1981194 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.0 g of 10,11-dihydro-5H-dibenzo[a,d]cycloheptene in 25 ml of dry tetrahydrofuran is treated dropwise at -70° with 6.8 ml of an about 1.14M solution of n-butyl lithium in hexane. The mixture is stirred at -70° for 60 minutes. There are subsequently added dropwise thereto at -30° 1.1 g of 2-chloroethylpyrrolidine in 2.5 ml of dry tetrahydrofuran and the mixture is stirred at -30° for 1 hour and at 0° to 5° for 3 hours. After evaporation of the mixture, the residue remaining is dissolved in toluene and washed with water. The organic phase is filtered over 10 g of aluminum oxide (activity grade II, neutral) using toluene for the elution. Crude 1-[2-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)ethyl]pyrrolidine is obtained as a yellow oil.

WORKUP

后处理

  1. additionThere are subsequently added dropwise
  2. customAfter evaporation of the mixture
  3. dissolutionthe residue remaining is dissolved in toluene
  4. washwashed with water
  5. filtrationThe organic phase is filtered over 10 g of aluminum oxide (activity grade II, neutral)
  6. washfor the elution