HRID372975

反应详情

EQUATION

反应方程式

HRID 372975 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-Ethoxybenzamidine (from sodium, 0.08 g, in ethanol, 10 ml, and 2-ethoxybenzamidine hydrochloride, 0.70 g) was dissolved in acetonitrile (10 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 (0.81 g) in acetonitrile (10 ml). The reaction mixture was stirred at 2° C. for one hour. Triethylamine (0.35 g) was added and the reaction mixture was stirred at ambient temperature for 21 hours to yield a white precipitate, 0.22 g, which was collected by filtration. The filtrate was reduced in volume under reduced pressure to yield a second crop of solid, 0.41 g. The products were combined and recrystallised from ethanol to yield the title compound, 0.30 g, m.p. 224.5°-225.5° C.

WORKUP

后处理

  1. additionwas added to
  2. temperaturea cooled
  3. stirringthe reaction mixture was stirred at ambient temperature for 21 hours
  4. customto yield a white precipitate, 0.22 g, which
  5. filtrationwas collected by filtration
  6. customto yield a second crop of solid, 0.41 g
  7. customrecrystallised from ethanol