HRID65029

反应详情

EQUATION

反应方程式

HRID 65029 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 40 ml of acetonitrile was dissolved 516 mg of thiourea. In the solution was suspended 2.5 g of 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)-ethanone hydrobromide. To the suspension was added dropwise slowly 0.95 ml of triethylamine while stirring. The mixture was stirred for 3 hours at a refluxing temperature, which was then left standing for cooling. Precipitating crystals were collected by filtration. The crystals were washed with an aqueous solution of saturated hydrogen carbonate, water, ethanol and ethylether in that order, followed by drying. The crystals were recrystallised from tetrahydrofuran to yield 1.5 g (90%) of 2-amino-4-(4-methoxyphenyl)-5-(3-pyridyl)-1,3-thiazol, m.p. 265°-266° C.

WORKUP

后处理

  1. stirringThe mixture was stirred for 3 hours at a refluxing temperature, which
  2. waitwas then left standing
  3. temperaturefor cooling
  4. customPrecipitating crystals
  5. filtrationwere collected by filtration
  6. washThe crystals were washed with an aqueous solution of saturated hydrogen carbonate, water, ethanol and ethylether in that order
  7. customby drying
  8. customThe crystals were recrystallised from tetrahydrofuran