反应详情

To the 2-(4′-tert-butylbiphenyl-3-yl)-9-hydroxy-3H-naphtho[1,2-d]imidazole-7-carboxylic acid (0.047 g, 0.1 mmol) in dimethylformamide (0.5 mL)at room temperature was added phenylalanine tert butyl ester hydrochloride (0.11 mmol). A cocktail solution of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.021 g, 0.11 mmol), triethylamine (0.3 mmol) in DMF (0.5 mL) was added and the reaction was agitated at room temperature for 18 hours. 1 ml water was added to the reaction mixture resulting in the formation of a tan precipitate. the mixture was filtered and allowed to dry. The solid mass was transferred into vial and dissolved in 1 ml of 90% trifluoroacetic acid. The solutions were agitated for 6 hrs then concentrated under reduced pressure. The residures were taked up in DMSO and subjected to Gilson HPLC purification. The title compound was abtained as solid.(0.016 g, 28%). MS(ES) m/z 584 [M+H].

1. customresulting in the formation of a tan precipitate
2. filtrationthe mixture was filtered
3. customto dry
4. dissolutiondissolved in 1 ml of 90% trifluoroacetic acid
5. stirringThe solutions were agitated for 6 hrs
6. concentrationthen concentrated under reduced pressure
7. customsubjected to Gilson HPLC purification