反应 #640573

反应方程式

water

3-[2-(Trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazinan-2-one

sodium hydrogen carbonate

propyl chloroformate

→

3-{2-[N-(propoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-[1,3]-oxazinan-2-one

收率 68.2%

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度heated
2. 2
   温度to reflux for six hours
3. 3
   萃取extracted with ethyl acetate
4. 4
   洗涤The organic layer was washed with a saturated brine
5. 5
   干燥dried over anhydrous sodium sulfate
6. 6
   其他the solvent was evaporated under reduced pressure
7. 7
   其他The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4)

实验过程

3-[2-(Trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazinan-2-one (0.13 g, 0.38 mmol) and sodium hydrogen carbonate (0.06 g, 0.71 mmol) was suspended in acetonitrile (15 ml), added with propyl chloroformate (0.09 g, 0.77 mmol) and heated to reflux for six hours. After cooling to room temperature, the reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with a saturated brine and then 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) to obtain 3-{2-[N-(propoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-[1,3]-oxazinan-2-one (0.11 g).

来源