反应详情

温度

-78 °C

A mixture of chlorzoxazone, 3-(t-butoxycarbonylamino)-1-propene, palladium diacetate, tritolylphosphine, and acetonitrile is cooled to −78° C., degassed, and sealed in a reaction tube. The mixture is kept at 50° C. with stirring for 60 hours, then cooled and opened and the acetonitrile removed under vacuum. The residue is dissolved in ethyl acetate and washed successively with 5% aqueous NaHCO3 and brine. After drying over Mg2SO4, the mixture is filtered and evaporated. Silica gel chromatography gives 5-(3-(t-butoxycarbonylamino)-1-propenyl)-2-benzoxazolone.

1. customdegassed
2. customsealed in a reaction tube
3. customis kept at 50° C.
4. temperaturecooled
5. customthe acetonitrile removed under vacuum
6. dissolutionThe residue is dissolved in ethyl acetate
7. washwashed successively with 5% aqueous NaHCO3 and brine
8. dry with materialAfter drying over Mg2SO4
9. filtrationthe mixture is filtered
10. customevaporated