反应详情

温度

70 °C

A mixture of 0.48 g (0.97 mmol) of ethyl 4-[benzyl-(4-methoxybenzenesulfonyl) amino]-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate and 0.29 ml of ION NaOH in 4 ml of tetrahydrofuran-methanol (1:1) was heated in an oil bath at 70° C. for 2 hours and the solvent removed under vacuum. The residue was dissolved in 20 ml of H2O and the solution extracted with 10 ml of diethyl ether. To the aqucous layer was added 2N citric acid (pH 4-5) and the precipitated solid filtered and washed with H2O to give a white solid which was dried under vacuum overnight to give crystals, mp 165-167° C.

1. customthe solvent removed under vacuum
2. dissolutionThe residue was dissolved in 20 ml of H2O
3. extractionthe solution extracted with 10 ml of diethyl ether
4. additionTo the aqucous layer was added 2N citric acid (pH 4-5)
5. filtrationthe precipitated solid filtered
6. washwashed with H2O
7. customto give a white solid which
8. customwas dried under vacuum overnight
9. customto give crystals, mp 165-167° C.