反应详情

温度

145 °C

A mixture of 40 g of N-cyclohexyl-3,3-dimethoxy-butyramide in 200 ml of toluene was stirred and heated to 145° C. to distill an azeotrope of toluene and methanol. After 3 hours, the mixture was cooled and evaporated to dryness under reduced pressure. The oil residue was chromatographed over silica gel and was eluted with a 7-3 methylene chlorideethyl acetate mixture. The fractions with an Rf of 0.55 were recovered and were concentrated to dryness under reduced pressure. The residue was added to isopropyl ether which was iced and vacuum filtered. The recovered precipitate was dried to obtain 18 g of N-cyclohexyl-3-methoxy-crotonamide melting at 109° C.

1. distillationto distill an azeotrope of toluene and methanol
2. temperaturethe mixture was cooled
3. customevaporated to dryness under reduced pressure
4. customThe oil residue was chromatographed over silica gel
5. washwas eluted with a 7-3 methylene chlorideethyl acetate mixture
6. customThe fractions with an Rf of 0.55 were recovered
7. concentrationwere concentrated to dryness under reduced pressure
8. additionThe residue was added to isopropyl ether which
9. filtrationvacuum filtered
10. customThe recovered precipitate was dried