HRID1995820
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringThe reaction mixture is stirred about 16 hours
- temperatureheated to 45° for about 30 minutes
- temperatureAfter cooling
- washwashed with water and saturated NaCl
- dry with materialdried (Na2SO4)
- washThe crystalline solid is washed with 20% ethyl acetate/hexane