HRID1768949

反应详情

EQUATION

反应方程式

HRID 1768949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 4-[3-[4-(1-adamantyl)-1-piperazinyl]-2-hydroxypropoxy]benzylcyanide (3.44 g, 8.4 mmol), 5-nitroso-2,4,6-triamino-pyrimidine (1.08 g, 7.0 mmol) and 0.2N sodium-(2-ethoxyethoxide) in 2-ethoxyethanol (35 ml) was stirred at 120° C. for 30 minutes. After cooling to about 90° C. 100 ml of water was added and the mixture was cooled to room temperature followed by stirring in an ice-water bath for 30 minutes. The precipitate was collected, washed with water and acetonitrile to give the title compound (3.23 g) as a yellow powder, mp. 287°-289° C. (dec.), yield: 84.6%.

WORKUP

后处理

  1. temperatureAfter cooling to about 90° C
  2. temperaturethe mixture was cooled to room temperature
  3. stirringby stirring in an ice-water bath for 30 minutes
  4. customThe precipitate was collected
  5. washwashed with water and acetonitrile