反应详情

30.75 g (0.15 mole) of 3-methyl-5-[2,6,6-trimethylcyclohex-1-en-1-yl]-isoxazole were dissolved in 50 ml of dry ethanol and the solution was added to 1.396 g of a mixture of 82.9 % of platinum oxide in 600 ml of ethanol, the said mixture having previously been subjected to a hydrogenation. The alcoholic solution was then subjected to a hydrogenation at ordinary temperature and pressure and, after absorption of one equivalent of hydrogen, was filtered through a Celite carrier. After having been concentrated under reduced pressure, the residual mixture was recrystallized from hexene containing traces of ethanol to yield 30.91 g (yield 100 %) of 2,6,6-trimethyl-1-[3-amino-but-2-enoyl]-cyclohex-1-ene which exists in two interconvertible crystalline structures: m.p. 124.5° - 125.0° and 135°-136°.

1. filtrationwas filtered through a Celite carrier
2. concentrationAfter having been concentrated under reduced pressure
3. customthe residual mixture was recrystallized from hexene containing traces of ethanol