反应详情

To a solution of 0.56 g (3.02 mmol) of 1-(2-naphthalenyl)ethanone oxime in 10 mL of DMF was added 0.13 g (3.28 mmol) of NaH. 0.75 (2.52 mmol) of the title compound of Step D was then added to the reaction and the mixture was stirred at room temperature for 3 h. The reaction mixture was washed successively with water and saturated NaCl and then extracted with ethyl acetate. The combined organic extracts were dried over magnesium sulfate, filtered, and concentrated. The crude product was purified by flash chromatography on silica gel using 60% ethyl acetate/hexane as eluent to give 0.80 g (79% yield) of the title compound of Step E, a compound of the invention, as a solid melting at 91-94° C.

1. washThe reaction mixture was washed successively with water and saturated NaCl
2. extractionextracted with ethyl acetate
3. dry with materialThe combined organic extracts were dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product was purified by flash chromatography on silica gel using 60% ethyl acetate/hexane as eluent