تفاعل #80290

معادلة التفاعل

ammonia

sulfolane

nitronium tetrafluoroborate

allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methylindol-4-carboxylate

→

desired compound

المردود 55.0%

Allyl 5-[(4,6-Dimethoxypyrimidin-2-yl)oxy]-2-methyl-3-nitroindol-4-carboxylate

المردود 55.0%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   أخرىwas returned to room temperature
2. 2
   استخلاصextracted with ethyl acetate
3. 3
   غسيلThe organic layer was washed with water
4. 4
   تجفيفdried over anhydrous sodium sulfate
5. 5
   أخرىCrystals obtained by concentration under reduced pressure
6. 6
   غسيلwere washed with hexane

الإجراء التجريبي

2.0 g of allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methylindol-4-carboxylate was dissolved in 25 ml of acetonitrile, and the solution was cooled to -30° C. 16.3 ml of a 0.5M sulfolane solution of nitronium tetrafluoroborate was dropwise added thereto, and the mixture was stirred for 5 hours. After adding 2 ml of aqueous ammonia, the mixture was returned to room temperature and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. Crystals obtained by concentration under reduced pressure, were washed with hexane to obtain 1.23 g (yield: 55%) of the desired compound.

المصدر