HRID542180

反应详情

EQUATION

反应方程式

HRID 542180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 35.2 g (0.20 mole) of 1-benzylpiperazine in 100 ml of CHCl3 was added dropwise over a period of 30 minutes a solution of 17.0 g (0.18 mole) of methyl chloroformate in 110 ml of CHCl3. The mixture was allowed to reflux during 2.5 hours and was made basic with 16 g of sodium hydroxide in 100 ml of water. The nonaqueous layer was separated, dried over magnesium sulphate and concentrated. The residue was distilled b.p. 108°-10° C. at 0.1-0.2 mmHg to give 34.5 g of 1-carbomethoxy-4-benzylpiperazine.

WORKUP

后处理

  1. temperatureto reflux during 2.5 hours
  2. customThe nonaqueous layer was separated
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated
  5. distillationThe residue was distilled b.p. 108°-10° C. at 0.1-0.2 mmHg