反应详情

A mixture of 10.5 g of ethyl thiocarbamate, 25.9 g of methyl 3-bromo-2-oxo-cyclohexanecarboxylate and 200 ml of dioxane was refluxed for 16 hours and was then distilled to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with a 1-1 cyclohexane-ethyl acetate mixture to obtain 4-carbomethoxy-2,3,4,5,6,7-hexahydrobenzothiazoline-2-one melting at 95° C.

1. temperaturewas refluxed for 16 hours
2. distillationwas then distilled to dryness under reduced pressure
3. customThe residue was chromatographed over silica gel
4. washwas eluted with a 1-1 cyclohexane-ethyl acetate mixture