تفاعل #8362

معادلة التفاعل

sodium bicarbonate

water

4-[2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinoline-1-oxide

trifluoroacetic anhydride

→

title compound

4-[2-(6-Methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-1H-quinolin-2-one

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   استخلاصThe mixture is extracted three times with ethyl acetate
2. 2
   غسيلthe combined organic extracts washed three times with water
3. 3
   تجفيفonce with brine, dried (sodium sulfate)
4. 4
   ترشيحfiltered
5. 5
   تركيزconcentrated in vacuo
6. 6
   أخرىThe residue is triturated with 10% acetone/90% dichloromethane
7. 7
   ترشيحfiltered
8. 8
   أخرىThe solid is dried under vacuum

الإجراء التجريبي

To a solution of 4-[2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinoline-1-oxide (103 mg, 0.30 mmol) in N,N-dimethylformamide (3 mL) is added trifluoroacetic anhydride (425 μL, 3.0 mmol). The mixture is stirred for 40 h, poured into water, and the pH adjusted to 8 with saturated aqueous sodium bicarbonate solution. The mixture is extracted three times with ethyl acetate, the combined organic extracts washed three times with water and once with brine, dried (sodium sulfate), filtered, and concentrated in vacuo. The residue is triturated with 10% acetone/90% dichloromethane and filtered. The solid is dried under vacuum to yield the title compound, 11.6 mg (10%), as a yellow solid.

المصدر