反应详情

A mixture of 23.8 g (0.104 mole) of 1-(4-chloro-3-nitrophenoxy)-2-propanone, 2 g of Raney nickel and 240 ml of dioxane is hydrogenated at normal pressure and room temperature. After 20 hours (hydrogen absorption: 103%), the whole is filtered with suction over Celite, then washed with dioxane and concentrated by evaporation in vacuo. Purification of the crude product by chromatographed with petroleum ether/ether over silica gel and subsequent recrystallisation from ether/petroleum ether yields 1-(3-amino-4-chlorophenoxy)-2-propanone having a melting point of 49°-51°.

1. customis hydrogenated at normal pressure and room temperature
2. customAfter 20 hours (hydrogen absorption: 103%)
3. filtrationthe whole is filtered with suction over Celite
4. washwashed with dioxane
5. concentrationconcentrated by evaporation in vacuo
6. customPurification of the crude product
7. customby chromatographed with petroleum ether/ether over silica gel and subsequent recrystallisation from ether/petroleum ether