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Organic Lab Reactions 302

Organic Lab Reactions 302 - ALKALINE FORMALDEHYDE...

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ALKALINE FORMALDEHYDE DEAMINATION 297 . Triptycene 8Si * from 2,5-Diaminotriptycene. One-half gram of sodium nitrite is added to 50 cc. of sulfuric acid (sp. gr. 1.84), and the mixture is stirred to effect complete solution. After cooling to —5° to 0°, 50 cc. of 50% hypophosphorous acid f (precooled to —5° to 0°) is added in about ten minutes. This is followed by a solution of 0.57 g. of 2,5-diaminotriptycene in 30 cc. of glacial acetic acid, approximately ten minutes being required for the addition. A temperature of —5° to 0° and gentle stirring are maintained for another three hours, after'which 100 g. of crushed ice is added, with vigorous stirring, over a period of ten to fifteen minutes. Stirring is continued for an additional ten min- utes, and the reaction mixture ^(loosely stoppered) is placed in the refrig- erator for twenty-four to thirty-six hours. The product is then poured into ice water, extracted with benzene, and washed with water, aqueous sodium hydroxide, and finally with water. After removal of the solvent, the residue is sublimed at 1 mm.
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