反应 #640571

反应方程式

water

triethylamine

triphosgene

3-(2-Nitrobenzylamino)-1-propanol

→

3-(2-nitrobenzyl)-[1,3]-oxazinan-2-one

收率 63.0%

溶剂

chloroform

反应条件

后处理

1. 1
   萃取extracted with ethyl acetate
2. 2
   洗涤after the organic layer was washed with a saturated brine, it
3. 3
   干燥was dried over anhydrous sodium sulfate
4. 4
   其他the solvent was evaporated under reduced pressure
5. 5
   其他The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4)

实验过程

3-(2-Nitrobenzylamino)-1-propanol (1.03 g, 4.90 mmol) was dissolved in chloroform (20 ml) and the reaction solution was cooled to 0° C. Then triethylamine (1.98 g, 19.6 mmol), triphosgene (0.58 g, 1.95 mmol) were added thereto and the mixture was stirred at the same temperature for 1.5 hours. The reaction mixture was added with water and extracted with ethyl acetate and after the organic layer was washed with a saturated brine, it was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4) and 3-(2-nitrobenzyl)-[1,3]-oxazinan-2-one (0.29 g) was obtained.

来源