HRID437051

反应详情

EQUATION

反应方程式

HRID 437051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 16.0 g of 2-chloroacetyl-1-(o-fluorobenzyl)pyrrole, Example 1a, 8.3 g of di-sec-butylamine and 20.0 g of potassium carbonate in 250 ml xylene is stirred at 120° C. for 72 hours. The mixture is cooled, washed with water, dried and filtered and the xylene is evaporated leaving a brown oil. The oil is dissolved in ether and extracted into a 2N hydrogen chloride solution. The aqueous acidic solution is basified with a sodium carbonate solution and extracted with ether. The ether solution is washed, dried and filtered and the ether removed leaving a brown oil of 1-(o-fluorobenzyl)-2[(di-sec-butylamino)acetyl]pyrrole. Infrared and nuclear magnetic resonance spectra confirm this structure.

WORKUP

后处理

  1. temperatureThe mixture is cooled
  2. washwashed with water
  3. customdried
  4. filtrationfiltered
  5. customthe xylene is evaporated
  6. customleaving a brown oil
  7. extractionextracted into a 2N hydrogen chloride solution
  8. extractionextracted with ether
  9. washThe ether solution is washed
  10. customdried
  11. filtrationfiltered
  12. customthe ether removed