تفاعل #640573

معادلة التفاعل

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

المردود 68.2%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated
2. 2
   درجة الحرارةto reflux for six hours
3. 3
   استخلاصextracted with ethyl acetate
4. 4
   غسيلThe organic layer was washed with a saturated brine
5. 5
   تجفيفdried over anhydrous sodium sulfate
6. 6
   أخرىthe solvent was evaporated under reduced pressure
7. 7
   أخرىThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4)

الإجراء التجريبي

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).

المصدر