反应详情

To a solution of [1-(4-bromophenyl)-2-(1-pyrrolidinyl)ethyl]methylamine (1.61 g, 5.68 mmol) and (6,7-dichloro-2-oxo-3,4-dihydro-1(2H)-quinolinyl)acetic acid (1.73 g, 6.25 mmol) in DMF (20 mL) was added BOP Reagent (3.77 g, 8.52 mmol) and triethylamine (1.72 g, 17.3 mmol). The resultant mixture was stirred at room temperature for 16 h. The mixture was concentrated under reduce pressure. The residue was diluted with ethyl acetate (100 mL) and extracted with 5% NaHCO3 (100 mL) and brine (100 mL). The organic layer was dried (MgSO4) and concentrated. The residue was purified by silica gel chromatography (120 g redisep column, silica 40 um, 60 A, 85 ml/min, A: MeOH, B: CH2Cl2, A: 1% for 20 min) to give 0.76 g (25%) title compound as yellow solid. MS (ES) m/e 545.4 [M+H]+.

1. concentrationThe mixture was concentrated
2. additionThe residue was diluted with ethyl acetate (100 mL)
3. extractionextracted with 5% NaHCO3 (100 mL) and brine (100 mL)
4. dry with materialThe organic layer was dried (MgSO4)
5. concentrationconcentrated
6. customThe residue was purified by silica gel chromatography (120 g redisep column, silica 40 um, 60 A, 85 ml/min