反应详情

To a solution of ethyl 6-cyclopropyl-1-(1,1-dimethylethyl)-3-methyl-1H-pyrazolo[3,4-b]pyridine-4-carboxylate (278 mg, 0.922 mmol) in ethanol (30 mL) was added sodium hydroxide (3.69 mL, 3.69 mmol) and the contents heated at reflux for 2 hours. The solvent was removed in vacuo, the residue dissolved in 20 mL of water, and acidifed by addition of acetic acid. The contents were extracted with EtOAc (4×30 ml). The combined organic extracts were washed with water, brine, dried over MgSO4, filtered, and concentrated in vacuo. The product was collected as 233 mg. 1H NMR (400 MHz, DMSO-d6) δ ppm 0.97-1.12 (m, 4 H), 1.69 (s, 9 H), 2.22-2.41 (m, 3 H), 2.52 (s, 3 H), 7.45 (s, 3 H). LCMS(ES) [M+H]+ 274.2

1. temperaturethe contents heated
2. temperatureat reflux for 2 hours
3. customThe solvent was removed in vacuo
4. dissolutionthe residue dissolved in 20 mL of water
5. additionacidifed by addition of acetic acid
6. extractionThe contents were extracted with EtOAc (4×30 ml)
7. washThe combined organic extracts were washed with water, brine
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo
11. customThe product was collected as 233 mg