By W. J. Criddle B.Sc., Ph.D., G. P. Ellis B.Sc., Ph.D., F.R.I.C. (auth.)
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Filter off the solid obtained. Recrystallize the product from water, aqueous ethanol or ethanol. g. 2,4,6-(N0 2 hC 6 H 2 ·0H + C 10 H 8 --+ [2,4,6-(N0 2 hC 6 H 2 ·0H][C 10 H 8 ] Prepare saturated solutions of either picric or styphnic acid and naphthalene in ethanol and mix. Warm gently for a few minutes and cool. A crystalline product is readily obtained which may be recrystallized from ethanol. g. ¢ 0 + 2H,N·OH ~ 0 ¢ N·OH + ~OH Prepare as described under Ketones, (p. 39). g. ¢ 0 + 2H,N·NH·CO·NH, ~ 0 Prepare as described under Aldehydes, (p.
Filter off the solid obtained. (iv) Dissolve the organic compound (0·5 g) in the minimum of glacial acetic acid and add a mixture of fuming nitric acid (2 ml) and glacial acetic acid (2 ml). Heat the mixture to boiling and allow to stand until cold. Pour into water (50 ml) and filter off the resulting solid. (v) As described in (iv) above but keep the mixture at 20° by cooling in ice. After standing for 5 minutes, dilute with water and filter off the solid product. In all the above cases, the crude product should be thoroughly washed with water and recrystallized from aqueous ethanol, ethanol or benzene.
Of dimedone (20 ml). A little ethanol may be added to dissolve the compound if necessary. If no precipitate forms within 2 minutes, warm the solution for 5 minutes, cool in ice and filter off the product. Recrystallize from aqueous ethanol or ethanol. AMIDES, IMIDES, UREAS AND GUANIDINES (a) Xanthyl derivative O(x) H RCO·NH 2 + OH 0 To the organic compound (0·5 g) add a 7% solution of xanthydrol in glaeial acetic acid (7 ml) and reflux for up to 30 minutes. Add water (5 ml) and allow to cool. Filter off the solid product and recrystallize from aqueous dioxan or acetic acid.