反应详情

温度

100 °C

A mixture of dehydro-aripiprazole (1.50 g, 3.36 mmol), triethylamine (1.03 mL, 7.39 mmol), diethyl carbamoyl chloride (1.02 mL) were combined in tetrahydrofuran (30 mL). This was then heated to 100° C. for 6 hours by microwave. The reaction was quenched with water (50 mL) and extracted with dichloromethane (2×100 mL). The combined organics were dried (MgSO4) and concentrated. The crude product was purified by column chromatrography on silica eluting with ethyl acetate to 20% tetrahydrofuran/ethyl acetate to give the product. The product was then triturated with heptane to remove aliphatic impurities and then dried to give Compound-334 (1.54 g) as a light brown oil.

1. customThe reaction was quenched with water (50 mL)
2. extractionextracted with dichloromethane (2×100 mL)
3. dry with materialThe combined organics were dried (MgSO4)
4. concentrationconcentrated
5. customThe crude product was purified by column chromatrography on silica eluting with ethyl acetate to 20% tetrahydrofuran/ethyl acetate
6. customto give the product
7. customThe product was then triturated with heptane
8. customto remove aliphatic impurities
9. customdried
10. customto give Compound-334 (1.54 g) as a light brown oil