HRID26439

反应详情

EQUATION

反应方程式

HRID 26439 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

155 G. of 2,4-diamino-6-chloropyrimidine-3-oxide are mixed and stirred under an argon atmosphere with 640 ml. of o-xylene and 260 ml. of 1,2,5,6-tetrahydropyridine. The mixture is then heated to reflux for 30 minutes, the internal temperature rising from 115° C. to 123° C. The mixture is then cooled to 5° C., treated with 40 g. of sodium hydroxide in 400 ml. of water and stirred at 5° C. for 1 hour. The precipitate formed is filtered off, washed with 200 ml. of water and recrystallized from 3000 ml. of water, there being obtained pure 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide having a melting point of 263°-265° C. (decomposition).

WORKUP

后处理

  1. temperatureThe mixture is then heated
  2. temperatureto reflux for 30 minutes
  3. customrising from 115° C. to 123° C
  4. additiontreated with 40 g
  5. customThe precipitate formed
  6. filtrationis filtered off
  7. washwashed with 200 ml
  8. customof water and recrystallized from 3000 ml