HRID1781404

反应详情

EQUATION

反应方程式

HRID 1781404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of sodium hydride (60% dispersion in mineral oil, 0.80 g, 20.0 mmol) in 15 mL dry dimethylformamide under argon, cooled in an ice-bath was added dropwise a solution of 2-imidazolidone (1.72 g, 20.0 mmol) in 5 mL dimethylformamide. The ice bath was removed, the mixture was stirred 30 minutes and a solution of 5'-chloromethyl-2'-hydroxyacetophenone (1.85 g, 10.0 mmol) in 5 mL dimethylformamide was added dropwise. The mixture was stirred four hours and the product was isolated in the same manner as in the previous example to give a solid. The solid was stirred under 20 mL n-butylchloride, filtered off, and dried in vacuo to give 1.01 g (43%) product as a white solid, mp 131°-133° C.

WORKUP

后处理

  1. temperaturecooled in an ice-bath
  2. customThe ice bath was removed
  3. stirringThe mixture was stirred four hours
  4. customto give a solid
  5. stirringThe solid was stirred under 20 mL n-butylchloride
  6. filtrationfiltered off
  7. customdried in vacuo