HRID597467

反应详情

EQUATION

反应方程式

HRID 597467 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12.2 g of 2-chloro-4-sec. butylamino-5-nitro-6-methylpyrimidine (0.05 mole) are dissolved in 200 ml of alcohol and 10 ml of triethylamine are added to this solution. The reaction mixture is heated to reflux temperature and then 4.5 g of methylmercaptan (0.094 mole) are passed in. Subsequently 1.2 g of sodium hydride (0.05 mole) are added at 70° C and the mixture is refluxed for 1 hour. After the reaction mixture has cooled, the sodium chloride precipitate is filtered off with suction and the filtrate is evaporated to yield 11.7 g of 2-methylthio-4-sec.butylamino-5-nitro-6-methylpyrimidine of m.p. 37°-41° C (= 91.5% yield). On recrystallisation from petroleum ether, the melting point of the product rises to 48°-50° C.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux temperature
  3. temperaturethe mixture is refluxed for 1 hour
  4. temperatureAfter the reaction mixture has cooled
  5. filtrationthe sodium chloride precipitate is filtered off with suction
  6. customthe filtrate is evaporated