HRID330379

反应详情

EQUATION

反应方程式

HRID 330379 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 4.2 g (0.03 mol) of 3-nitrophenol in 150 ml of acetone is added 7.5 g (0.05 mol) of 2-chloromethyl-6-phenylpyridine hydrochloride3, 10 g (0.03 mol) of cesium carbonate and 0.5 g of potassium iodide, and the slurry is heated to reflux for 20 hours. The hot mixture is filtered, and the filtrate is concentrated in vacuo to obtain an oil (9.3 g). The crude product is recrystallized from ethyl acetate/pentane to give a first crop (4.5 g, 49%) of crystals, m.p. 77°-80° C. and a second crop (1.7 g, 19%) of crystals, m.p. 77°-81° C.

WORKUP

后处理

  1. temperaturethe slurry is heated
  2. temperatureto reflux for 20 hours
  3. filtrationThe hot mixture is filtered
  4. concentrationthe filtrate is concentrated in vacuo