HRID1700363

反应详情

EQUATION

反应方程式

HRID 1700363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

32 g of the product obtained in Step A are heated at reflux in a solution of 400 ml of toluene and 35 ml of POCl3. After 3 hours, the reaction mixture is concentrated under reduced pressure, the residue is taken up in 300 ml of ethanol, and 5 g of sodium borohydride are slowly added. After 30 minutes, 300 ml of water are added and the ethanol is distilled off. After extraction of the residue with dichloromethane, drying and evaporation under reduced pressure, the oily residue obtained is converted into the hydrochloride in an ethanolic hydrogen chloride solution. The expected product is isolated by filtration and drying in vacuo.

WORKUP

后处理

  1. concentrationthe reaction mixture is concentrated under reduced pressure
  2. addition5 g of sodium borohydride are slowly added
  3. waitAfter 30 minutes
  4. addition300 ml of water are added
  5. distillationthe ethanol is distilled off
  6. extractionAfter extraction of the residue with dichloromethane
  7. customdrying
  8. customevaporation under reduced pressure
  9. customthe oily residue obtained