HRID1768946

反应详情

EQUATION

反应方程式

HRID 1768946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

A mixture of 2,6-diamino-4-chloropyrimidine (0.43 g, 3.0 mmol) and 1-(1-adamantyl)-piperazine (0.66 g, 3.0 mmol) in ethanol (30 ml) was heated in a sealed tube at 170° C. for 3 hours. After cooling the solvent was removed, the solid residue was dissolved in water (45 ml) and acidified to pH=3 with conc. HCl. The obtained mixture was heated to 50° C. the insolubles were filtered off and the clear solution was rendered alkaline with 10N NaOH under stirring and cooling. The precipitated crystals were collected, washed with water until neutral and dried. In this manner 0.79 g of the title compound was obtained in the form of its monohydrate, yield: 76.6%, mp. 265°-268° C.

WORKUP

后处理

  1. temperatureAfter cooling the solvent
  2. customwas removed
  3. dissolutionthe solid residue was dissolved in water (45 ml)
  4. temperatureThe obtained mixture was heated to 50° C. the insolubles
  5. filtrationwere filtered off
  6. temperaturecooling
  7. customThe precipitated crystals were collected
  8. washwashed with water until neutral and
  9. customdried