反应详情

To a solution of aripiprazole (1.5 g, 3.35 mmol) in dichloromethane (33 mL) was added triethylamine (0.56 mL, 4.01 mmol) and ethyl isocyanate (0.53 mL, 6.69 mmol). The reaction was stirred at room temperature for 5 days. The reaction was quenched with water and extracted with dichloromethane (3×20 mL). The organics were combined, washed with saturated aqueous sodium hydrogen carbonate (20 mL) and brine (20 mL), dried over MgSO4 and concentrated. The product was purified by column chromatography on silica eluting with 0-3% methanol in 1:1 ethyl acetate to dichloromethane. The product was triturated in heptane to remove aliphatic impurities and then filtered and dried. The material was dissolved in ethyl acetate and washed with saturated aqueous sodium hydrogen carbonate (6×15 mL) to afford Compound-72 (0.482 g) as a pink solid.

1. customThe reaction was quenched with water
2. extractionextracted with dichloromethane (3×20 mL)
3. washwashed with saturated aqueous sodium hydrogen carbonate (20 mL) and brine (20 mL)
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customThe product was purified by column chromatography on silica eluting with 0-3% methanol in 1:1 ethyl acetate to dichloromethane
7. customThe product was triturated in heptane
8. customto remove aliphatic impurities
9. filtrationfiltered
10. customdried
11. dissolutionThe material was dissolved in ethyl acetate
12. washwashed with saturated aqueous sodium hydrogen carbonate (6×15 mL)
13. customto afford Compound-72 (0.482 g) as a pink solid