反应详情

To a solution of 4,4-dimethyl-7-[2-([1,7]naphthyridin-2-ylamino)-benzoylamino]-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (Step B, 200 mg, 0.38 mmol) in EtOAC (2 mL) was added concentrated HCl in EtOAc (5 mL). The mixture was stirred for 5 h at RT under N2 atmosphere. The solid was filtered off and dissolved in water. The aqueous solution was basified to pH 11-14 using 5N NaOH. The solution was extracted with EtOAc, and the organic layer was dried over Na2SO4. The volatiles were removed under reduced pressure and the crude was purified with flash chromatography (SiO2, 5% MeOH/CH2Cl2) to obtain the desired compound as a white solid. MS (ES+): 424.0 (M+H)+. Calc'd for C26H25N5O-423.51.

1. filtrationThe solid was filtered off
2. dissolutiondissolved in water
3. extractionThe solution was extracted with EtOAc
4. dry with materialthe organic layer was dried over Na2SO4
5. customThe volatiles were removed under reduced pressure
6. customthe crude was purified with flash chromatography (SiO2, 5% MeOH/CH2Cl2)