反应 #1880970

反应方程式

N-(2,3-epoxypropyl)phthalimide

sodium azide

ammonium chloride

→

desired product

收率 92.9%

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

收率 92.9%

溶剂

DMF

反应条件

后处理

1. 1
   温度The reaction mixture was cooled to room temperature
2. 2
   过滤filtered
3. 3
   其他The filtrate was evaporated to dryness
4. 4
   workup.DISSOLUTIONThe residue was dissolved in benzene (800 ml)
5. 5
   洗涤washed with water, brine and water sequentially
6. 6
   干燥dried over sodium sulfate
7. 7
   其他The solvent was removed in vacuo
8. 8
   其他The desired product was further purified by silica gel chromatography

实验过程

To DMF solution (400 ml) of N-(2,3-epoxypropyl)phthalimide 58.8 g (0.29 mol), sodium azide 37.6 g (0.58 mol) and ammonium chloride 18.5 g (0.35 mol) were added, and stirred at 90° C. for 3 hours. The reaction mixture was cooled to room temperature, and then filtered. The filtrate was evaporated to dryness. The residue was dissolved in benzene (800 ml), washed with water, brine and water sequentially and then dried over sodium sulfate. The solvent was removed in vacuo. The desired product was further purified by silica gel chromatography. 66.3 g of desired product was obtained. The NMR spectra were consistent with the desired title intermediate.

来源