반응 #8362

반응 방정식

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

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   추출The mixture is extracted three times with ethyl acetate
2. 2
   세척the combined organic extracts washed three times with water
3. 3
   건조once with brine, dried (sodium sulfate)
4. 4
   여과filtered
5. 5
   농축concentrated in vacuo
6. 6
   기타The residue is triturated with 10% acetone/90% dichloromethane
7. 7
   여과filtered
8. 8
   기타The solid is dried under vacuum

실험 절차

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.

출처