反应详情

The 2-[2,4-dioxo-3-(1-tert-butyloxycarbonyl-1H-indazol-3-ylmethylene)-5-phenyl-2,3,4,5-tetrahydro-1H-1,5-diazepin-1-yl]-N-isopropyl-N-(4-methoxyphenyl)acetamide (170 mg) was dissolved in CHCl3 (10 ml) and TFA (5 ml) was added. The reaction mixture was stirred for 6 hrs and the solvents were removed in vacuo. The crude product was purified by RP HPLC Dynamax (C-8) (10 ml/min (50% Acetonitrile, 50% Water (0.1% TFA), followed by lyophilization, to afford the titled product of Example 1 (135 mg) as a white lyophilate. HPLC Column: Dynamax C-8 2 ml/min., 30-70% Acetonitrile in aqueous TFA (0.1% v/v) over 20 min., Tr=17.1 min. 1H NMR (400 MHz, CDCl3) 7.93 (d, J=8.3 Hz, 1H), 7.59 (m, 2H), 7.11 (m, 2H), 7.31 (m, 6H), 6.93 (m, 2H), 6.00 (s, 2H), 4.92 (sept., J=6.3 Hz, 1H), 4.15 (m, 1H), 3.92 (m, 4H), 3.82 (s, 3H), 1.04 (d, J=6.3 Hz, 6H), MS (FAB) [M+H]+=538.

1. customthe solvents were removed in vacuo
2. customThe crude product was purified by RP HPLC Dynamax (C-8) (10 ml/min (50% Acetonitrile, 50% Water (0.1% TFA)