HRID1995820

反应详情

EQUATION

反应方程式

HRID 1995820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-hydroxy-2-nitropyridine (7 g), K2CO3 (6.9 g) of DMF (100 ml) is stirred for about 10 minutes. To the mixture is added 4-chlorobenzyl chloride (8.1 g) in portions over about 15 minutes. The reaction mixture is stirred about 16 hours and then heated to 45° for about 30 minutes. After cooling, the reaction is diluted with CHCl3, washed with water and saturated NaCl, dried (Na2SO4) and stripped. The crystalline solid is washed with 20% ethyl acetate/hexane, giving 5-(4-chlorobenzyloxy)-2-nitropyridine.

WORKUP

后处理

  1. stirringThe reaction mixture is stirred about 16 hours
  2. temperatureheated to 45° for about 30 minutes
  3. temperatureAfter cooling
  4. washwashed with water and saturated NaCl
  5. dry with materialdried (Na2SO4)
  6. washThe crystalline solid is washed with 20% ethyl acetate/hexane