HRID1578932

反应详情

EQUATION

反应方程式

HRID 1578932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 38.4 g (0.164 mole) 1-bromo-2-naphthaldehyde, 16.4g (0.164 mole) triethylamine, and 30.6 g (0.164 mole) of 2-amino-1-phenyl-1-propanol hydrochloride in 500 ml CH3OH was stirred and refluxed for 60 minutes, then cooled to 10°-20° while 6.23 g (0.164 mole) of sodium borohydride was added over 5 minutes. The reaction mixture was stirred at ambient temperature (15°-21°) for 60 minutes and diluted with 500 ml H2O. The mixture was stirred for 15 minutes and extracted with 2 × 350 ml CHCl3. The combined extracts were dried (MgSO4) and concentrated to dryness in vacuo to give 59.6 g (99%) of the free base.

WORKUP

后处理

  1. temperaturerefluxed for 60 minutes
  2. additionwas added over 5 minutes
  3. stirringThe reaction mixture was stirred at ambient temperature (15°-21°) for 60 minutes
  4. stirringThe mixture was stirred for 15 minutes
  5. extractionextracted with 2 × 350 ml CHCl3
  6. dry with materialThe combined extracts were dried (MgSO4)
  7. concentrationconcentrated to dryness in vacuo