反应详情

温度

110 °C

The product from Example 68A (52 mg, 0.212 mmol) was treated with 1,4,7-triazonane trihydrochloride (202 mg, 0.847 mmol), treated with Hunig's base (554 μl, 3.17 mmol), treated with 2-methoxyethanol (2116 μl), stirred at 110° C. for 19 hours, cooled, diluted with Et2O (25 mL), washed with 0.1 M NaOH (2×10 mL), washed with brine, dried (MgSO4), filtered, concentrated and purified by chromatography on silica gel (eluting with 2, 10 and 50% (9:1 MeOH:concentrated NH4OH) in CH2Cl2) to provide the title compound. 1H NMR (CD3OD) δ 2.08-2.24 (m, 2H), 2.40 (t, J=6.94 Hz, 2H), 2.67 (t, J=6.74 Hz, 2H), 2.94 (s, 4H), 3.10-3.16 (m, 4H), 3.71-3.77 (m, 4H), 7.24-7.29 (m, 1H), 7.32-7.41 (m, 2H), 7.63-7.68 (m, 1H); MS (M+H)+ m/z 339.

1. temperaturecooled
2. washwashed with 0.1 M NaOH (2×10 mL)
3. washwashed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified by chromatography on silica gel (eluting with 2, 10 and 50% (9:1 MeOH:concentrated NH4OH) in CH2Cl2)