反应详情

To a solution of the product of Step 3 in THF (150 mL), was added cyanoacetic acid (870 mg, 10.2 mmol), EDC (4.32 g, 22.5 mmol) and triethylamine (8 ml, 51 mmol). This mixture was then stirred at rt for overnight. The reaction mixture was concentrated, taken up in EtOAC (300 mL), washed with saturated NaHCO3 solution and brine, dried over Na2SO4, filtered and concentrated. The residue was dissolved in AcOH (100 ml), and then heated to 115° C. for 24 h. The reaction mixture was concentrated to afford the title compound, which was used directly to next step without further purification. MS (ES+) m/e 309 [M+H]+.

1. concentrationThe reaction mixture was concentrated
2. washwashed with saturated NaHCO3 solution and brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. dissolutionThe residue was dissolved in AcOH (100 ml)
7. temperatureheated to 115° C. for 24 h
8. concentrationThe reaction mixture was concentrated