反应详情

温度

-20 °C

A slurry of 5-amino-3-dodecylisoxazole (1.44 g, 5.71 mmol) in acetonitrile (50 mL) was warmed until homogeneous. 2,6-Diisopropylphenylisocyanate (1.22 mL, 5.71 mmol) was then added in one portion and the resulting solution was heated under reflux for 24 hours. The resulting solution was cooled to -20° C. The resulting precipitate was collected by filtration, dissolved in a minimal amount of warm chloroform, and chromatographed on silica (70:30 hexane:ethyl acetate). The product containing fractions were concentrated and the resulting solid was recrystallized from acetonitrile to yield 0.53 g (20.4%) of the title compound as white needles, m.p. 112.5°-114° C.

1. temperaturethe resulting solution was heated
2. temperatureunder reflux for 24 hours
3. filtrationThe resulting precipitate was collected by filtration
4. dissolutiondissolved in a minimal amount of warm chloroform
5. customchromatographed on silica (70:30 hexane:ethyl acetate)
6. additionThe product containing fractions
7. concentrationwere concentrated
8. customthe resulting solid was recrystallized from acetonitrile