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
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This note was uploaded on 11/20/2011 for the course CHM 2210 taught by Professor Reynolds during the Fall '01 term at University of Florida.

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