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a-Phenyltrifluoroacetylacetonitrile hydrate (245g ) was added to a mixture of 425 g. of 98% sulfuric acid and 250 cc. of water in a flask equipped with a dropping funnel and a 30-cm. unpacked insulated column. The mixture was heated to 160 and steam distillation from the top of the column began at 95-98 . Water was added slowly from the dropping funnel at such a rate that the volume remained constant. The temperature rose slowly and was maintained at 100-110 by adjusting the rate of addition of water. After six hours the mixture darkened and the distillate no longer gave a precipitate with 28% ammonium hydroxide. The disttillate was extracted with ether and the extract dried over sodium sulfate and fractionated.The colorless liquid ketone boiled at 51-52(2 mm.) .It weighed 146g (73%) [ Last edited by lwl913 on 2008-12-17 at 10:31 ] |
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