HRID1031172

反应详情

EQUATION

反应方程式

HRID 1031172 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 2-chlorobenzimidazole (25 g, 0.165 mol) and 3-methylamino-1-methylpyrrolidine (72 g, 0.63 mol) was heated at 120° C. with an oil bath for 18 hr. After cooling, 500 ml of 2.5N NaOH solution was added and the mixture extracted twice with 100 ml portions of methylene chloride. The methylene chloride extracts were combined and washed successively with 2×100 ml portions of 2.5N NaOH solution and 3×100 ml portions of water. The methylene chloride solution was dried (Na2SO4) and concentrated to obtain 15 g of product (40% yield).

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionthe mixture extracted twice with 100 ml portions of methylene chloride
  3. washwashed successively with 2×100 ml portions of 2.5N NaOH solution and 3×100 ml portions of water
  4. dry with materialThe methylene chloride solution was dried (Na2SO4)
  5. concentrationconcentrated