反应详情

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0 °C

A 17.4 gm. portion of 2-phenyl-4-imidazolemethanol and 13.4 ml. of concentrated HNO3 are heated on a steam bath for 21/2 hours. Three drops of fuming HNO3 are added to start the reaction. The pH is adjusted to 8 with concentrated aqueous Na2CO3 and the mixture is cooled to 0° C. overnight. The solid is recovered, washed with water and recrystallized from a mixture of 70 ml. of ethyl acetate and 20 ml. of petroleum ether giving a yellow solid. Treatment of the mother liquor with petroleum ether gives an additional tacky substance which is triturated with isopropanol giving a second solid. These two solids are taken up in hot isopropanol and recrystallized as a yellow solid. This solid is recrystallized from ethanol:water (1:1) giving yellow crystals, m.p. 169°-171.5° C.

1. customthe reaction
2. customThe solid is recovered
3. washwashed with water
4. customrecrystallized from a mixture of 70 ml
5. customTreatment of the mother liquor with petroleum ether gives an additional tacky substance which
6. customis triturated with isopropanol giving a second solid
7. customrecrystallized as a yellow solid
8. customThis solid is recrystallized from ethanol:water (1:1)
9. customgiving yellow crystals, m.p. 169°-171.5° C.