反应详情

A mixture of 77 g of ethyl 2-chloromethyl-5-ethylnicotinate (0.338 mol), 44 g of α-methylvalinamide (0.338 mol) and 33.5 g of sodium bicarbonate (0.4 mol) in 60 mL dimethylsulfoxide is stirred and heated at 80° for 16 hours. The reaction is partitioned between 1:1 ethylacetate-hexane and water. The organic layer is washed thoroughly with water, dried, and concentrated in vacuo to a gum. Chromatography of this gum on silica gel using hexane-ethyl acetate mixtures as eluant affords the title product, mp 68°-72°.

1. temperatureheated at 80° for 16 hours
2. customThe reaction is partitioned between 1:1 ethylacetate-hexane and water
3. washThe organic layer is washed thoroughly with water
4. customdried
5. concentrationconcentrated in vacuo to a gum