反应详情

温度

120 °C

To a 330-mL pressure vessel was added 2-(2-(4-((6-chloro-3-pyridinyl)sulfonyl)-2-(1-propyn-1-yl)-1-piperazinyl)-5-pyrimidinyl)-1,1,1-trifluoro-2-propanol (6.50 g, 13.3 mmol), EtOH (80 mL), and ammonium hydroxide (30%, 80.0 mL, 616 mmol, J. T. Baker, Philipsburg, N.J.). The tube was sealed and heated at 120° C. for 10 h and then the solvent was removed in vacuo. The residue was partitioned between water (100 mL) and DCM (200 mL). The aqueous layer was extracted with DCM (2×100 mL) and the combined organic extracts were dried over MgSO4, filtered, and concentrated. The crude product was purified by column chromatography (330 g of silica, 1 to 5% 2 M NH3 in MeOH in DCM) to afford 2-(2-(4-((6-amino-3-pyridinyl)sulfonyl)-2-(1-propyn-1-yl)-1-piperazinyl)-5-pyrimidinyl)-1,1,1-trifluoro-2-propanol (5.0 g) as a mixture of four isomers.

1. customThe tube was sealed
2. customthe solvent was removed in vacuo
3. customThe residue was partitioned between water (100 mL) and DCM (200 mL)
4. extractionThe aqueous layer was extracted with DCM (2×100 mL)
5. dry with materialthe combined organic extracts were dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude product was purified by column chromatography (330 g of silica, 1 to 5% 2 M NH3 in MeOH in DCM)