HRID5510

反应详情

EQUATION

反应方程式

HRID 5510 的结构方程式

CONDITIONS

反应条件

温度
225 °C

PROCEDURE

实验过程

To a mixture of 1.3 g of sodium hydride (in the form of a 60% by weight suspension in mineral oil) and 100 g (0.64 mol) of ethyl 1-pyrrolidineacetate was added 91 g of 2-(1-pyrrolidinyl)ethanol. The mixture was heated slowly to about 225° C., and the ethanol by-product was collected in a Dean-Stark trap. The reaction mixture was cooled to about 25° C., then 12 g of 1-bromopropane was added to react any alkoxide present. The sodium bromide by-product was removed by filtration. The desired product 2-(1-pyrrolidinyl)ethyl 1-pyrrolidineacetate was purified by distillation at 95° C. at a pressure of 250 μmHg. The structural assignment was confirmed by mass spectral analysis.

WORKUP

后处理

  1. customthe ethanol by-product was collected in a Dean-Stark trap
  2. temperatureThe reaction mixture was cooled to about 25° C.
  3. addition12 g of 1-bromopropane was added
  4. customto react any alkoxide present
  5. customThe sodium bromide by-product was removed by filtration
  6. distillationThe desired product 2-(1-pyrrolidinyl)ethyl 1-pyrrolidineacetate was purified by distillation at 95° C. at a pressure of 250 μmHg