反応 #8362

反応方程式

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

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   抽出The mixture is extracted three times with ethyl acetate
2. 2
   洗浄the combined organic extracts washed three times with water
3. 3
   乾燥once with brine, dried (sodium sulfate)
4. 4
   ろ過filtered
5. 5
   濃縮concentrated in vacuo
6. 6
   その他The residue is triturated with 10% acetone/90% dichloromethane
7. 7
   ろ過filtered
8. 8
   その他The solid is dried under vacuum

実験手順

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.

出典