反应详情

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.

1. extractionThe mixture is extracted three times with ethyl acetate
2. washthe combined organic extracts washed three times with water
3. dry with materialonce with brine, dried (sodium sulfate)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue is triturated with 10% acetone/90% dichloromethane
7. filtrationfiltered
8. customThe solid is dried under vacuum