反应详情

Diisopropylethylamine (0.35 g, 2.7 mmole) was added in one portion to a stirred mixture of bis [2-(4-pyridyl)ethyl]amine (0.37 g, 1.65 mmole), methyl (±)-7-carboxy-4-methyl-3-oxo-2,3,4,5-tetrahydro-1H-1,4-benzodiazepine-2-acetate (0.44 g, 1.50 mmole), EDC (0.34 g, 1.8 mmole), and HOBT . H2O (0.24 g, 1.8 mmole) in DMF (8 mL) at 0° C. under argon, and the reaction was allowed to warm to RT. After 19.5 h, the reaction was poured into a mixture of ice water (100 g) and 5% NaHCO3 (10 mL) and extracted with CH2Cl2 (2×100 mL). The combined organic layers were washed with 5% NaHCO3 (50 mL), dried (MgSO4), and concentrated. Chromatography on silica gel (7% MeOH/CH2Cl2) gave the title compound (0.7 g, 88%). MS (ES) m/e 502.4 (M+H)+. c) (±)-7-[[Bis[2-(4-pyridinyl)ethyl]amino]carbonyl]-4-methyl-3-oxo-2,3,4,5-tetrahydro-1H-1,4-benzodiazepine-2-acetic acid

1. customat 0° C.
2. extractionextracted with CH2Cl2 (2×100 mL)
3. washThe combined organic layers were washed with 5% NaHCO3 (50 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated