反应详情

A mixture of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-carboxyphenyl)benzamide (232 mg), diphenylphosphoryl azide (151 mg), and triethylamine (0.084 ml) in benzene (10 ml) was refluxed for 5 hours and 1N hydrochloric acid (4 ml) was added to the solution. The mixture was refluxed for 4 hours and the mixture was washed with aqueous saturated sodium hydrogen carbonate and brine. The organic solution was dried over magnesium sulfate and the solvent was evaporated in vacuo to give crude oil. The oil was purified by silica gel column (10 g, 2% methanol in chloroform) and the product was solidified with diethyl ether to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-aminophenyl)benzamide (120 mg).

1. temperaturewas refluxed for 5 hours
2. temperatureThe mixture was refluxed for 4 hours
3. washthe mixture was washed with aqueous saturated sodium hydrogen carbonate and brine
4. dry with materialThe organic solution was dried over magnesium sulfate
5. customthe solvent was evaporated in vacuo
6. customto give crude oil
7. customThe oil was purified by silica gel column (10 g, 2% methanol in chloroform)