反应详情

温度

50 °C

The product of step c) (300 mg), the product of step d) (219 mg) and potassium carbonate (135 mg) in acetonitrile (10 ml) were charged to a flask and stirred at 50° C. for 16 h. The reaction mixture was cooled, diluted with water (20 ml) and extracted with diethyl ether (3×10 ml). The organic fractions were washed with brine, dried (MgSO4) and concentrated in vacuo. The resulting yellow oil was dissolved in a 1:1 mixture of THF/methanol (10 ml) and 1M NaOH added (1.1 ml). The mixture was stirred at room temperature for 4 h and then concentrated in vacuo. The residue was purified by RPHPLC to give the title compound as a white solid (175 mg).

1. temperatureThe reaction mixture was cooled
2. extractionextracted with diethyl ether (3×10 ml)
3. washThe organic fractions were washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. dissolutionThe resulting yellow oil was dissolved in a 1:1 mixture of THF/methanol (10 ml) and 1M NaOH
7. additionadded (1.1 ml)
8. stirringThe mixture was stirred at room temperature for 4 h
9. concentrationconcentrated in vacuo
10. customThe residue was purified by RPHPLC