HRID1153758

反应详情

EQUATION

反应方程式

HRID 1153758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A mixture of 1.6 gm (5.2 mmols) of diethyl 2-amino-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine-3,7-dicarboxylate and 20 ml of 80% sulfuric acid was heated for 30 minutes at 180° C. Thereafter, the mixture was cooled, made alkaline with an aqueous sodium carbonate solution, and extracted with chloroform for 24 hours with a perforator. The chloroform extract was chromatographed in silicagel with chloroform/methanol/concentrated ammonia (24:12:1) as the mobile phase.

WORKUP

后处理

  1. temperatureThereafter, the mixture was cooled
  2. extractionextracted with chloroform for 24 hours with a perforator
  3. extractionThe chloroform extract
  4. customwas chromatographed in silicagel with chloroform/methanol/concentrated ammonia (24:12:1) as the mobile phase