反应详情

温度

-10 °C

(1H-Imidazol-4-yl)-(6-methoxynaphthalen-2-yl)ketone (6.50 g) was dissolved in THF (120 ml) and the mixture was cooled to −10° C. A solution (2.0 M; 38.7 ml) of isopropyl magnesium chloride in THF was slowly added dropwise and the mixture was stirred for 30 min. To the reaction mixture was added saturated aqueous solution of ammonium chloride and the mixture was diluted with water and extracted with ethyl acetate. The extract was washed with saturated brine, and after drying, concentrated. The obtained residue was purified by silica gel column chromatography (eluate, chloroform:methanol=20:1→10:1) and recrystallized from ethyl acetate to give the title compound (5.04 g) as a colorless crystalline powder.

1. extractionextracted with ethyl acetate
2. washThe extract was washed with saturated brine
3. customafter drying
4. concentrationconcentrated
5. customThe obtained residue was purified by silica gel column chromatography (eluate, chloroform:methanol=20:1→10:1)
6. customrecrystallized from ethyl acetate