反应 #1880971

反应方程式

hydrogen

N-(3-azido-2-hydroxypropyl)phthalimide

hydrochloric acid

→

desired product

N-(3-Amino-2-hydroxypropyl)phthalimide hydrochloride

溶剂

ethanol

反应条件

后处理

1. 1
   其他After removal of catalyst
2. 2
   过滤by filtration, catalyst
3. 3
   洗涤was washed with EtOH/DMF (1:1) solution (300 ml)
4. 4
   其他combined filtrate was evaporated to dryness
5. 5
   workup.ADDITIONAddition of EtOH to the residue

实验过程

To ethanol solution (240 ml) of N-(3-azido-2-hydroxypropyl)phthalimide 10 g (40.3 mol), 10% Pd—C (1 g) and concentrated hydrochloric acid solution 7.84 ml (80.6 mmol) were added sequentially. To the reaction mixture, hydrogen was introduced at 2 kgf/cm2 atm. and hydrogenated at room temperature for 6 hours. After removal of catalyst by filtration, catalyst was washed with EtOH/DMF (1:1) solution (300 ml) and then combined filtrate was evaporated to dryness. Addition of EtOH to the residue gave crystal of desired product as hydrogen chloride salt. Crystal was collected by filtration and dried under reduced pressure at 40° C. to afford 5.3 g of the product. The NMR spectra were consistent with the desired title intermediate.

来源