HRID2263365

反应详情

EQUATION

反应方程式

HRID 2263365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butyl 4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxylate (5.06 g, 14.6 mmol) in ethyl acetate (80 ml) was added a 4 N solution of hydrogen chloride in ethyl acetate (40 ml), and the mixture was stirred at room temperature for 5 hours. Hexane (200 ml) was added to the reaction mixture and a precipitated solid was collected by filtration. The obtained solid was added to an aqueous saturated sodium bicarbonate solution (300 ml), followed by stirring at room temperature for 2 hours. The obtained powder was collected by filtration to yield 2.77 g (77.0%) the desired product.

WORKUP

后处理

  1. filtrationa precipitated solid was collected by filtration
  2. additionThe obtained solid was added to an aqueous saturated sodium bicarbonate solution (300 ml)
  3. stirringby stirring at room temperature for 2 hours
  4. filtrationThe obtained powder was collected by filtration