تفاعل #41691

معادلة التفاعل

nitric acid

N-(4-(1-acetylpyrrolidin-2-yl)-3-fluorophenyl)pyrazine-2-carboxamide

sodium bicarbonate

→

N-(4-(1-acetylpyrrolidin-2-yl)-5-fluoro-2-nitrophenyl)pyrazin-2-carboxamide

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwith cooling with ice
2. 2
   أخرىthe reaction liquid
3. 3
   أخرىThe reaction liquid
4. 4
   استخلاصextracted with chloroform
5. 5
   غسيلThe organic layer was washed with saturated saline
6. 6
   تجفيفdried with anhydrous magnesium sulfate
7. 7
   أخرىThe solvent was evaporated away under reduced pressure
8. 8
   أخرىthe resulting residue was purified through silica gel column chromatography (developing solvent: chloroform/methanol=50/1)
9. 9
   أخرىto obtain the entitled compound as a yellow oily substance

الإجراء التجريبي

40 ml of fuming nitric acid was added to 3.9 g of N-(4-(1-acetylpyrrolidin-2-yl)-3-fluorophenyl)pyrazine-2-carboxamide with cooling with ice, and the reaction liquid was stirred at room temperature for 2 hours. The reaction liquid was diluted with water with ice, made basic with aqueous saturated sodium bicarbonate, and then extracted with chloroform. The organic layer was washed with saturated saline, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: chloroform/methanol=50/1) to obtain the entitled compound as a yellow oily substance.

المصدر