反应详情

To a solution of 5.0 g (11.7 mmol) of compound 8c in 20 ml of acetone, 3.3 g (23.4 mmol) of methyl iodide were added and the mixture was refluxed under stirring for 6 hrs, then cooled. The orange crystalline solid which separated was filtered, washed with ether and crystallized for acetone/ether. Yield, 5.6 g (85%), m.p. 163°-165° C. U.V. (buffer pH 7.4) 270, 215 nm. NMR (DMSO-d6) δ 7.68-7.06 (ms, 7H, C5N4N+ +C6H3 +NH), 4.56 (s, 3H, --N+ --CH3), 3.42 (q, 2H, J=7 Hz, --N--CH2), 3.19 (t, 2H, J=7 Hz, CH2), 1.32 (s, 18H, 2 --C(CH3)3). Anal. Calcd for C25H33IN2O5 : C, 52.82; H, 5.85; N, 4.92. Found: C, 52.76; H, 5.87; N, 4.90.

1. temperaturethe mixture was refluxed
2. temperaturecooled
3. customThe orange crystalline solid which separated
4. filtrationwas filtered
5. washwashed with ether
6. customcrystallized for acetone/ether
7. customYield