反应详情

温度

100 °C

To a solution of COMPOUND 249 (0.1882 g, 0.61 mmol) in 1,4-dioxane (25 mL) was added sulfamide (0.5826 g, 6.06 mmol), and stirred at 100° C. for 4 hours. The mixture was concentrated and water (20 mL) was added and extracted with CH2Cl2 (2×75 mL). The combined organic extracts were washed with water (2×30 mL), dried (Na2SO4), filtered and concentrated. Purification of the crude material by column chromatography on silica gel (33:1:1 CH2Cl2-MeOH—NH4OH) provided 0.1461 g (59%) of COMPOUND 342 as a white solid. 1H NMR (CDCl3) δ 1.80-1.88 (m, 2H), 1.95-2.00 (m, 2H), 2.08 (s, 6H), 2.48-2.58 (m, 3H), 3.76-3.82 (m, 6H), 4.76 (s, 2H), 7.06-7.11 (m, 2H), 7.37 (d, 2H, J=7.2 Hz), 8.33 (d, 2H, J=3.0 Hz).

1. concentrationThe mixture was concentrated
2. additionwater (20 mL) was added
3. extractionextracted with CH2Cl2 (2×75 mL)
4. washThe combined organic extracts were washed with water (2×30 mL)
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification of the crude material by column chromatography on silica gel (33:1:1 CH2Cl2-MeOH—NH4OH)