反应详情

温度

125 °C

To 250 mg (0.79 mmol) of efavirenz 1 was added 10 mL of anhydrous DMF, 600 mg (4.34 mmol) of potassium carbonate, 120 mg (0.80 mmol) of sodium iodide and 492 mg (2.2 mmol) of 4-bromo-butyric acid tert-butyl ester followed by 5 mg of 18-crown-6. The mixture was heated to 125° C. for 2 hours under argon atmosphere and concentrated under reduced pressure. To the residue 50 mL of chloroform was added, and the solid was filtered off. To the filtrate 50 mL of water was added. The organic layer was separated, washed with 50 mL of water, dried (Na2SO4), and concentrated. The residue was purified by silica gel flash column chromatography in 70% ethyl acetate in hexane to give 327 mg (0.721 mmol, 90% yield) of 2 (M+Na, 480).

1. concentrationconcentrated under reduced pressure
2. additionTo the residue 50 mL of chloroform was added
3. filtrationthe solid was filtered off
4. additionTo the filtrate 50 mL of water was added
5. customThe organic layer was separated
6. washwashed with 50 mL of water
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated
9. customThe residue was purified by silica gel flash column chromatography in 70% ethyl acetate in hexane