HRID1879466

反应详情

EQUATION

反应方程式

HRID 1879466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (S)-2-amino-N,N-dimethyl-3-phenyl-propionamide (1.0 g, 5.2 mmol) in tetrahydrofuran (10 mL) was added a solution of lithium aluminum hydride in tetrahydrofuran and toluene (3.5 M, 7.4 mL, 26 mmol) dropwise. The mixture was heated to reflux for 4 h after addition and then cooled. Ether (20 mL) was added. Ethyl acetate was added dropwise until all the lithium aluminum hydride was consumed. Sodium hydroxide (1M, 20 mL) was added and the mixture was stirred for 30 min. The mixture was extracted three times with ether. The combined organic extracts were washed with brine, dried over sodium sulfate and evaporated to give (S)—N1,N1-dimethyl-3-phenyl-propane-1,2-diamine (0.60 g, 65%)

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 4 h
  3. additionafter addition
  4. temperaturecooled
  5. customwas consumed
  6. additionSodium hydroxide (1M, 20 mL) was added
  7. extractionThe mixture was extracted three times with ether
  8. washThe combined organic extracts were washed with brine
  9. dry with materialdried over sodium sulfate
  10. customevaporated