反应详情

To a solution of 1-benzyl-3-(4-chloro-phenyl)-1,4,5,6,7,8-hexahydro-1,2,6-triaza-azulene (Example 59, Step E; 1 mmol) in acetone (3 mL) was added Na2CO3 (2 mmol) and bromoacetic methyl ester (2 mmol). The mixture was stirred at RT for 1 h. After concentration and purification (SiO2, 2 M NH3 in MeOH/CH2Cl2), the title compound was obtained (60 mg). MS (ESI): exact mass calculated for C23H24ClN3O2, 409.16. found, m/z 410.1 [M+H]+. 1H NMR (500 MHz, CDCl3): 7.44-7.42 (m, 2H), 7.31-7.29 (m, 2H), 7.25-7.23 (br m, 2H), 7.20-7.18 (br m, 1H), 7.02-6.99 (br m, 2H), 5.26 (s, 2H), 3.64 (s, 2H), 3.41 (s, 2H), 2.81-2.79 (br m, 4H), 2.75-2.73 (br m, 2H), 2.70-2.68 (br m, 2H).

1. concentrationAfter concentration and purification (SiO2, 2 M NH3 in MeOH/CH2Cl2)