HRID9723

反应详情

EQUATION

反应方程式

HRID 9723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.643 g 4-Amino-N-methylphthalimide was suspended in 50 ml THF and added to 1.328 g lithium aluminum hydride in 50 ml THF at room temperature. The mixture was refluxed for 3 hrs, then stirred a further 3 days at room temperature. Excess LAH was destroyed by addition of water and the mixture filtered over celite. An aqueous phase was separated and extracted with CH2Cl2. The combined organic phases were dried and evaporated. The residue was stirred with HCl in MeOH and the evaporated to yield 1.6 g of the title compound as the hydrochlorid salt.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 3 hrs
  2. customExcess LAH was destroyed by addition of water
  3. filtrationthe mixture filtered over celite
  4. customAn aqueous phase was separated
  5. extractionextracted with CH2Cl2
  6. customThe combined organic phases were dried
  7. customevaporated
  8. stirringThe residue was stirred with HCl in MeOH
  9. customthe evaporated