反应详情

温度

50 °C

Oxalyl chloride (218 mg, 1.72 mmol) is slowly added to a solution of 2-(4-(((benzyloxycarbonyl)(methyl)-amino)methyl)phenyl)benzo[d]oxazole-4-carboxylic acid (0.65 g, 1.57 mmol) in dichloromethane (10 mL) with stirring. The reaction mixture is warmed to 50° C. for 4 h and then cooled to 25° C. The solution is condensed in vacuum and then slowly added to 28% NH4OH (6 mL). The mixture is warmed to 50° C. and stirred for another 2 h. Water (50 mL) is added to the reaction mixture and the slurry is cooled to 25° C. The product is filtered and the cake is washed with water, dried to afford benzyl 4-(4-carbamoylbenzo[d]oxazol-2-yl)benzyl(methyl)carbamate solid. MS (ESI) m/e 416 [M+H]+.

1. temperaturecooled to 25° C
2. customcondensed in vacuum
3. temperatureThe mixture is warmed to 50° C.
4. stirringstirred for another 2 h
5. temperaturethe slurry is cooled to 25° C
6. filtrationThe product is filtered
7. washthe cake is washed with water
8. customdried