反应详情

To 4.0 g of 2-amino-3-cyano-4-(1,1-dimethylethyl)furan and 4.3 g of 2-methyl-4-chlorobutyryl chloride was added 150 ml of toluene. The reaction mixture was allowed to reflux for about 72 hours. The mixture was washed once with 1N hydrochloric acid, once with 2N sodium hydroxide and finally with water. The organic phase was dried over anhydrous magnesium sulfate, filtered and concentrated under vacuum. The residue was chromatographed over silica gel while eluting with an 80/20 mixture of Skellysolve B/ethyl acetate. Fractions containing the major component were combined and the solvent was evaporated therefrom to afford 1.3 g of N-[3-cyano-4-(1,1-dimethylethyl)-2-furyl]-3-methyl-2-pyrrolidinone. mp=88°-90° C. Yield 21%.

1. temperatureto reflux for about 72 hours
2. washThe mixture was washed once with 1N hydrochloric acid, once with 2N sodium hydroxide and finally with water
3. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. customThe residue was chromatographed over silica gel
7. washwhile eluting with an 80/20 mixture of Skellysolve B/ethyl acetate
8. additionFractions containing the major component
9. customthe solvent was evaporated