HRID12493

反应详情

EQUATION

反应方程式

HRID 12493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Under N2 atmosphere, 1-(4-chloro-phenyl)-3-dimethylamino-propan-1-one hydrochloride (37.2 g) was dissolved in warm MeOH (75 mL), and slowly added to a solution of hydrazine hydrate (23 mL) and 50% aqueous NaOH (12 mL) in MeOH (30 mL) stirred at 50° C. The mixture was refluxed for 2 hours, and evaporated under reduced pressure. Water was added to the residue, followed by extraction with DCM. The organic phase was washed twice with water, dried and evaporated under reduced pressure, to give 25.0 g of a yellow solid, m.p. 90-100° C.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2 hours
  2. customevaporated under reduced pressure
  3. additionWater was added to the residue
  4. extractionfollowed by extraction with DCM
  5. washThe organic phase was washed twice with water
  6. customdried
  7. customevaporated under reduced pressure