反应详情

Following the procedure described in Example 3(B), Step B, 3-{6-[(benzyl-isopropyl-carbamoyl)-methyl]-5-oxo-1-phenyl-5,6-dihydro-4H-2,3,6,10b-tetraaza-benzo[e]azulen-4-ylmethyl}-indazole-1-carboxylic acid tertbutyl ester (19.1 mg, 0.274 mmol) was deprotected with HCl (4.0M in dioxane, 0.8 mL) over 24 hours. The reaction was diluted with EtOAc, and the organic solution was washed with aqueous NaHCO3 (1×), dried (Na2SO4), filtered and concentrated. Purification by preparative chromatography eluting with 5% MeOH in CH2Cl2 provided 8.5 mg of N-benzyl-2-[4-(1H-indazol-3-ylmethyl)-5-oxo-1-phenyl-4,5-dihydro-2,3,6,10b-tetraaza-benzo[e]azulen-6-yl]-N-isopropyl-acetamide as a racemic mixture. 1H NMR (CD2Cl2) δ 7.97 (t, 1H), 7.12-7.64 (m, 15H), 7.05 (m, 1H), 6.92 (m, 1H), 5.08 (d) and 4.81 (d, total 1H), 4.60-4.74 (m, 2H), 4.49 (s, 1H), 4.45 (t, 1H), 4.29-4.39 (m, 1H), 3.96-4.13 (m, 2H), 1.16 (dd, 3H), 1.05 (dd, 3H); MS 596.2 (M+1), 594.2 (M−1).

1. washthe organic solution was washed with aqueous NaHCO3 (1×)
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customPurification by preparative chromatography
6. washeluting with 5% MeOH in CH2Cl2