反应详情

温度

60 °C

A mixture of 38 g of thiobutyramide, 54.2 g of ethyl 2-formyl-2-chloro-acetate, 185 ml of dioxane and 22 g of magnesium carbonate was heated for 4 hours at 60°C and the precipitate formed was removed by filtration. The dioxane was distilled from the filtrate and the residue was taken up in 665 ml of a 1-1 ethyl ether-water mixture. The ether phase was recovered by decantation and was washed with aqueous 10% hydrochloric acid solution and then with water until the wash waters were neutral, dried over magnesium sulfate and distilled to dryness. The residue was distilled to obtain 57 g of ethyl 2-n-propylthiazol-5-carboxylate boiling at 95°-106°C under 0.5 mm Hg.

1. customthe precipitate formed
2. customwas removed by filtration
3. distillationThe dioxane was distilled from the filtrate
4. customThe ether phase was recovered by decantation
5. washwas washed with aqueous 10% hydrochloric acid solution
6. dry with materialdried over magnesium sulfate
7. distillationdistilled to dryness
8. distillationThe residue was distilled