HRID1248890

反应详情

EQUATION

反应方程式

HRID 1248890 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

11.8 g (0.1 mole) of α-methoxy-isobutyric acid were dissolved in 150 ml of tetrahydrofuran, and 10.1 g (0.1 mole) of triethylamine were added. 10.85 g (0.1 mole) of carbonic acid ethyl ester-chloride were added dropwise at 10°-15° C., with stirring. The mixture was subsequently stirred at room temperature for 2 hours and 23.1 g (0.1 mole) of 2-(4-aminophenylmercapto)-4,6-dimethyl-pyrimidine were then added in portions. The mixture was subsequently stirred at room temperature for 1 hour and boiled under reflux for a further 2 hours. The reaction mixture was cooled and then stirred into one liter of water rendered slightly acid with hydrochloric acid. The crystals precipitated were filtered off with suction, washed with water and dried in air. 27.4 g (83% of theory) of 2-(4-(α-methoxy-isobutyrylamino)-phenylmercapto)-4,6-dimethyl-pyrimidine were obtained.

WORKUP

后处理

  1. stirringThe mixture was subsequently stirred at room temperature for 2 hours
  2. stirringThe mixture was subsequently stirred at room temperature for 1 hour
  3. temperatureunder reflux for a further 2 hours
  4. temperatureThe reaction mixture was cooled
  5. customThe crystals precipitated
  6. filtrationwere filtered off with suction
  7. washwashed with water
  8. customdried in air