反应详情

温度

0 °C

A 0° C. solution of the product of Example 46B (1.9 g, 8.6 mmol) in anhydrous dimethylformamide (10 mL) was treated portion-wise with 60% sodium hydride (410 mg, 10 mmol) in mineral oil. The reaction mixture was stirred twenty minutes at 0° C., and methyl iodide (1.4 mL, 22 mmol) was then added. Ice bath was removed, and reaction mixture stirred 16 hours at room temperature. Reaction mixture quenched with saturated ammonium chloride, and product extracted with ethyl acetate (2×). The combined extracts were washed with water and brine, dried (Na2SO4), filtered, and concentrated under reduced pressure. Residue purified by normal phase HPLC on silica gel eluting with 3% ethyl acetate/hexane to provide the title compound.

1. customIce bath was removed
2. customreaction mixture
3. stirringstirred 16 hours at room temperature
4. customReaction mixture
5. customquenched with saturated ammonium chloride, and product
6. extractionextracted with ethyl acetate (2×)
7. washThe combined extracts were washed with water and brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure
11. customResidue purified by normal phase HPLC on silica gel eluting with 3% ethyl acetate/hexane