反应详情

A solution of 5.32 g of methyl 1,4-dimethoxy-2-naphthoate [prepared as described in step (a) above] in 15 ml of tetrahydrofuran was added dropwise to a suspension of 0.98 g of lithium aluminum hydride in 15 ml of tetrahydrofuran, whilst ice-cooling. The resulting mixture was then stirred at room temperature for 1 hour, after which 20 ml of a saturated aqueous solution of ammonium chloride was added. The precipitate which formed was filtered off, and then the product was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and then concentrated by evaporation under reduced pressure, to give 3.97 g of the title compound as a pale yellow solid, melting at 63°-66° C.

1. temperaturecooling
2. customThe precipitate which formed
3. filtrationwas filtered off
4. extractionthe product was extracted with ethyl acetate
5. dry with materialThe extract was dried over anhydrous sodium sulfate
6. concentrationconcentrated by evaporation under reduced pressure