反应详情

Stannous chloride dihydrate (15.8 g, 0.07 mol) is added to a solution of 1-(4-cyclohexyl-3-nitrophenyl)ethanone (5.8 g, 0.0235 mol) in concentrated hydrochloric acid (35 mL) at 0-5° C. The reaction mixture is slowly brought to 60-65° C. and is stirred at this temperature for 15 minutes. After cooling to room temperature the reaction mixture is extracted with ethyl acetate (3×100 mL). The pH is adjusted to 8.0-9.0 using solid sodium bicarbonate. After washing with water (1×15 mL) the organic layer is dried over sodium sulfate and concentrated under reduced pressure to yield the crude, which is purified by column chromatography (230-400 mesh; ethyl acetate:n-hexane, 3:7) to give 1-(3-amino-4-cyclohexylphenyl)ethanone.

1. customis slowly brought to 60-65° C.
2. extractionis extracted with ethyl acetate (3×100 mL)
3. washAfter washing with water (1×15 mL) the organic layer
4. dry with materialis dried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customto yield the crude, which
7. customis purified by column chromatography (230-400 mesh; ethyl acetate:n-hexane, 3:7)