反应 #640579

反应方程式

water

6-Methyl-3-[2-(trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazepan-2-one

sodium hydrogen carbonate

isobutyl chloroformate

→

3-(2-[N-(isobutoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-6-methyl-[1,3]-oxazepan-2-one

收率 52.3%

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
   洗涤The ethyl acetate 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=3:1)

实验过程

6-Methyl-3-[2-(trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazepan-2-one (0.15 g, 0.41 mmol) and sodium hydrogen carbonate (0.06 g, 0.71 mmol) were suspended in acetonitrile (10 ml), added with isobutyl chloroformate (00.10 g, 0.73 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 ethyl acetate 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=3:1) to obtain 3-(2-[N-(isobutoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-6-methyl-[1,3]-oxazepan-2-one (0.10 g).

来源