HRID372976

反应详情

EQUATION

反应方程式

HRID 372976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2 °C

PROCEDURE

实验过程

2-Methoxybenzamidine (from sodium, 0.15 g, in ethanol, 20 ml, and 2-methoxybenzamidine methanesulphonate, 1.70 g) was dissolved in acetonitrile (20 ml) and the resulting cooled (2° C.) solution was added to a cooled (2° C.) suspension of ethyl 4-chloro-2-methylthio-5-pyrimidine carboxylate (2.33 g) in acetonitrile (20 ml). Triethylamine (0.66 g) was added and the reaction mixture was stirred at 2° C. for one hour and at ambient temperature for 18 hours. Acetonitrile was removed under reduced pressure and water (25 ml) was added. The mixture was cooled and a white solid was collected, washed with water and recrystallised from ethanol to yield the title compound, 0.46 g, m.p. 229°-231° C. (dec.).

WORKUP

后处理

  1. additionwas added to
  2. temperaturea cooled
  3. customAcetonitrile was removed under reduced pressure and water (25 ml)
  4. additionwas added
  5. temperatureThe mixture was cooled
  6. customa white solid was collected
  7. washwashed with water
  8. customrecrystallised from ethanol