HRID1578932
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturerefluxed for 60 minutes
- additionwas added over 5 minutes
- stirringThe reaction mixture was stirred at ambient temperature (15°-21°) for 60 minutes
- stirringThe mixture was stirred for 15 minutes
- extractionextracted with 2 × 350 ml CHCl3
- dry with materialThe combined extracts were dried (MgSO4)
- concentrationconcentrated to dryness in vacuo