反应详情

A mixture of 1.34 g (2.7 mmol) of ethyl 4-[(4-methoxy-benzenesulfonyl)pyridin-3-ylmethylamino]-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridin-5-carboxylate, 2.97 ml of 1N potassium hydroxide in 7.8 ml of ethanol and 4.83 ml of water was refluxed for 20 hr. Another 0.54 ml of 1N potassium hydroxide was added and the mixture refluxed 4 hrs. The solvent was removed under vacuum and toluene added and removed under vacuum. The residue was dissolved in water (20 ml) and extracted with ethyl acetate. The aqueous layer was acidified with 2 N citric acid and the precipitated solid filtered off and washed with water. The solid was dried under vacuum to give 0.98 g of solid, mp 256-258° C.

1. temperaturewas refluxed for 20 hr
2. temperaturethe mixture refluxed 4 hrs
3. customThe solvent was removed under vacuum and toluene
4. additionadded
5. customremoved under vacuum
6. dissolutionThe residue was dissolved in water (20 ml)
7. extractionextracted with ethyl acetate
8. filtrationthe precipitated solid filtered off
9. washwashed with water
10. customThe solid was dried under vacuum