HRID260153

反应详情

EQUATION

反应方程式

HRID 260153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To 250 mL of 2N HCl was added 8.0 g (55 mmoles) of 4,6-diaminopyrimidine hydrochloride (34). The 4,6-diamino-pyrimidine hydrochloride was allowed to dissolve. The solution was then cooled to 0° C. and a solution of 4.2 g (61 mmoles) of NaNO2 dissolved in 15 mL of H2O was added dropwise within 20 minutes while stirring. Stirring was continued for another 30 minutes at 0° and then 2 hours at room temperature. The violet solution was neutralized by NaHCO3, the precipitate collected, washed with H2O and ethanol and dried to give 35 as 6.3 g (82% yield) of a blue-violet crystal powder (m.p. >350° C.).

WORKUP

后处理

  1. dissolutionto dissolve
  2. additionwas added dropwise within 20 minutes
  3. stirringStirring
  4. custom2 hours
  5. customat room temperature
  6. customthe precipitate collected
  7. washwashed with H2O and ethanol
  8. customdried