HRID704898

反应详情

EQUATION

反应方程式

HRID 704898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(2-Methoxyphenyl)piperazine (22.6 g, 0.118 mol) and atropic acid (17.4 g, 0.118 mol) in ethanol (300 mL) were heated under reflux for 18 hours, cooled to room temperature, and evaporated in vacuo. The solid was triturated with acetone (3×100 mL) to give a first crop of 3-[4-(2-methoxyphenyl)piperazinyl]-2-phenylpropionic acid (13.8 g) as white crystals. The filtrate was evaporated in vacuo to give an oil which slowly crystallized over 1 month. The solid was triturated with acetone (200 mL) to give a second crop of the same hemihydrate product (9.01 g) as white crystals, mp. 160°-163° C.

WORKUP

后处理

  1. temperatureunder reflux for 18 hours
  2. customevaporated in vacuo
  3. customThe solid was triturated with acetone (3×100 mL)