反应详情

tert-Butyl (1-(4-(1-(cyanomethyl)-6-oxo-8-phenyl-1,6-dihydropyrano[3,2-g]indazol-7-yl)phenyl)cyclobutyl)carbamate (20 mg, 0.037 mmol) was loaded in a 1 g SCX-2 cartridge column preconditioned with methanol (2×1 mL). The compound was loaded to the column using 1 mL of methanol. After 1 h the column was washed with 3×1 mL of methanol. The product was eluted with 7 N ammonia in methanol (2×1 mL). The solvent was evaporated to afford the title compound (6 mg, 49%). Residual starting material was recovered from MeOH washed (10 mg). 1H NMR (500 MHz, MeOD): δ 8.19 (br s, 1H), 8.06 (d, J=8.6 Hz, 1H), 7.71 (d, J=8.3 Hz, 1H), 7.50-7.47 (m, 2H), 7.40-7.30 (m, 5H), 7.25-7.20 (m, 2H), 5.65 (s, 2H) 5.12 (s, 1H, NH) 2.64-2.56 (m, 4H), 2.30-2.22 (m, 1H), 2.04-1.94 (m, 1H). LCMS (Method J): RT=0.92 min, [M+H]+=448.

1. washAfter 1 h the column was washed with 3×1 mL of methanol
2. washThe product was eluted with 7 N ammonia in methanol (2×1 mL)
3. customThe solvent was evaporated