HRID66554

反应详情

EQUATION

反应方程式

HRID 66554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 42 g (0.219 m) of the phenylacetonitrile 100 ml of tetrahydrofuran was mixed with 400 ml of 1 molar diborane in tetrahydrofuran then heated at reflux for 21/2 hours. After cooling the mixture was quenched with 150 ml of methanol. After sitting overnight, the mixture was stripped. An excess of 10% hydrochloric acid was added followed by heating on the steambath for 2 hours. After cooling, ether was added. The mixture was stirred for 1/2 hour and evaporated. The remaining aqueous layer was made basic with 10% sodium hydroxide, extracted with ether which was dried and evaporated to give 2-methyl-3,4-dimethoxyphenethylamine.

WORKUP

后处理

  1. temperaturethen heated
  2. temperatureat reflux for 21/2 hours
  3. temperatureAfter cooling the mixture
  4. customwas quenched with 150 ml of methanol
  5. additionAn excess of 10% hydrochloric acid was added
  6. temperatureby heating on the steambath for 2 hours
  7. temperatureAfter cooling
  8. additionether was added
  9. customevaporated
  10. extractionextracted with ether which
  11. customwas dried
  12. customevaporated