HRID597465

反应详情

EQUATION

反应方程式

HRID 597465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15 ml of triethylamine are added to a solution of 15.6 g of 2,4-dichloro-5-nitro-6-methylpyrimidine (0.075 mole) in 300 ml of absolute ethanol. With ice cooling, 6.6 g of sec. butylamine (0.09 mole) are added dropwise at 0°-5° C over the course of c. 40 minutes to the dark red solution. After the mixture has been stirred for c. 3/4 hour at this temperature, it is poured into c. 700 ml of ice water and the water is extracted 3 times with ether. The ethereal extracts are dried over magnesium sulphate and evaporated. The resultant red oily substance is crystallised from petroleum ether to yield 10.5 g of 2-chloro-4-sec. butylamino-5-nitro-6-methyl-pyrimidine of m.p. 40°-43° C.

WORKUP

后处理

  1. custom40 minutes
  2. addition3/4 hour at this temperature, it is poured into c
  3. extraction700 ml of ice water and the water is extracted 3 times with ether
  4. dry with materialThe ethereal extracts are dried over magnesium sulphate
  5. customevaporated
  6. customThe resultant red oily substance is crystallised from petroleum ether