反应详情

A solution of 1-oxo-2,3,4,5-tetrahydro-1H-[1,4]diazepino[1,2-a]benzimidazole-8-carboxylic acid (Intermediate B, 59 mg, 0.15 mmol) and TBTU (52 mg, 0.16 mmol) in DMF (2 mL) is stirred for 20 min at room temperature. 3-(1-Tritylimidazol-4-yl)-aniline (Intermediate O, 36 mg, 0.15 mmol) and triethylamine (15 mg, 0.15 mmol) are added and the solution stirred at room temperature for 4 h. DMAP (5 mg, 0.04 mmol) is added and the solution is heated at 60° C. overnight. The reaction is cooled to room temperature and H2O was added. The resulting precipitate is filtered off and purified via flash column chromatography using a gradient elution of 0-10% CH2Cl2/methanol, containing 1% NH4OH to afford the title compound as an oil (67 mg, 73%).

1. temperaturethe solution is heated at 60° C. overnight
2. temperatureThe reaction is cooled to room temperature
3. filtrationThe resulting precipitate is filtered off
4. custompurified via flash column chromatography
5. washa gradient elution of 0-10% CH2Cl2/methanol
6. additioncontaining 1% NH4OH