反应详情

Add potassium carbonate (21 mg, 0.15 mmol) to a solution of 1-benzenesulfonyl-3-[2-(pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-1H-pyrrolo[2,3-b]pyridine (Example 3, Part A; 34 mg, 0.77 mmol) in methanol/water (0.9 mL/0.3 mL). Reflux the reaction overnight (16 h). Concentrate in vacuo, add aqueous sodium chloride (10 mL), and extract with chloroform (3×25 mL). Dry the combined organic extracts with sodium sulfate, filter, and concentrate in vacuo. Purify by flash column chromatography, using the appropriate mixture of methylene chloride, chloroform, methanol, and concentrated aqueous ammonium hydroxide, to provide 16 mg (68%) of the title compound as an off-white solid. MS (ES) m/z=302 (M+H).

1. temperatureReflux
2. customthe reaction overnight (16 h)
3. concentrationConcentrate in vacuo
4. additionadd aqueous sodium chloride (10 mL)
5. extractionextract with chloroform (3×25 mL)
6. dry with materialDry the combined organic extracts with sodium sulfate
7. filtrationfilter
8. concentrationconcentrate in vacuo
9. customPurify by flash column chromatography
10. additionthe appropriate mixture of methylene chloride, chloroform, methanol, and concentrated aqueous ammonium hydroxide