反应详情

To a mixture of 4-(t-butoxycarbonylaminomethyl)benzoic acid (3.77 g), L-phenylalamine amide hydrochloride (3.01 g), triethylamine (2.25 g) and dry dichloromethane (100 ml) 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (3.16 g) was added, under ice-cooling, and after cooling for 2 hours, the mixture was stirred under room temperature for 2 hours. The solvent was evaporated under a reduced pressure, water was added to the residue to effect powdering, and the powder was collected by filtration. The powder was washed with 10% aqueous citric acid, water, 5% aqueous sodium hydrogen carbonate, and then water, in this order, followed by drying, to give N-[4-(t-butoxycarbonylaminomethyl)benzoyl]-L-phenylalamine amide (I) (4.41 g). The structure was confirmed by NMR spectrum.

1. additionwas added, under ice-
2. temperaturecooling
3. temperatureafter cooling for 2 hours
4. customThe solvent was evaporated under a reduced pressure, water
5. additionwas added to the residue to effect powdering
6. filtrationthe powder was collected by filtration
7. washThe powder was washed with 10% aqueous citric acid, water, 5% aqueous sodium hydrogen carbonate
8. customby drying