反应 #1880973

反应方程式

hydrogen

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

hydrochloric acid

→

desired product

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

溶剂

EtOH

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 (60 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 EtOH solution (80 ml) of N-(3-azido-2(R)-hydroxypropyl)phthalimide 1.96 g (7.69 mmol), 10% Pd—C (200 mg) and concentrated hydrochloric acid solution 1.4 ml were added sequentially. To the reaction mixture, hydrogen was introduced at 2 kgf/cm2 atm. and then stirring was continued at room temperature overnight. After removal of catalyst by filtration, catalyst was washed with EtOH/DMF (1:1) solution (60 ml) and then combined filtrate was evaporated to dryness. Addition of EtOH to the residue gave crystal of desired product as a hydrogen chloride salt. Crystal was collected by filtration and dried under reduced pressure at 40° C. to afford 1.28 g of the product. The NMR spectra were consistent with the desired title intermediate.

来源