HRID597468

反应详情

EQUATION

反应方程式

HRID 597468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10 ml of triethylamine are added to a solution of 15.9 g of 2-chloro-4-sec. butylamino-5-nitro-6-methylpyrimidine (0.065 mole) in 250 ml of alcohol. Then 4.5 g (0.1 mole) of dimethylamine are passed in and the mixture is boiled for 4 hours at 100° C. After it has cooled, the mixture is evaporated and the residue is suspended in water. The resultant precipitate is filtered off with suction and washed with water until no more chlorine ions are dissolved out. The product is dried in a water jet vacuum at 50° C to yield 16.2 g of 2-dimethylamino-4-sec. butylamino-5-nitro-6-methylpyrimidine (=98.5% yield) of m.p. 98°-100° C. On recrystallisation from petroleum ether, the melting point of the product rises to 109°-110° C.

WORKUP

后处理

  1. temperatureAfter it has cooled
  2. customthe mixture is evaporated
  3. filtrationThe resultant precipitate is filtered off with suction
  4. washwashed with water until no more chlorine ions
  5. dissolutionare dissolved out
  6. dry with materialThe product is dried in a water jet vacuum at 50° C