反应 #640582

反应方程式

water

5,5-dimethyl-3-[2-(trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazinan-2-thione

sodium hydrogen carbonate

methyl chloroformate

→

5,5-dimethyl-3-(2-[N-(methoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-[1,3]-oxazinane-2-thione

收率 46.6%

溶剂

acetonitrile

反应条件

后处理

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

实验过程

5,5-dimethyl-3-[2-(trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazinan-2-thione (0.15 g, 0.39 mmol) and sodium hydrogen carbonate (0.05 g, 0.60 mmol) were suspended in acetonitrile (10 ml), added with methyl chloroformate (0.06 g, 0.60 mmol) and heated to reflux for three hours. After cooling to room temperature, the reaction mixture was added with water and extracted with ethyl acetate. The solvent was evaporated under reduced pressure after the organic layer was dried over anhydrous sodium sulfate. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:l) to obtain 5,5-dimethyl-3-(2-[N-(methoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-[1,3]-oxazinane-2-thione (0.08 g).

来源