Cyclobutanone oxime

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Ethyl 5-fluoro-6-hydroxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate (6.60 g., 30 mmoles), acetic anhydride (3.27 g., 32 mmoles), pyridine (10 ml.) and acetone (10 ml.) were mixed and allowed to stand overnight at ordinary temperature (18°-23° C.). To this mixture were added cyclobutanone oxime (3.82 g., 45 mmoles) and pyridine (5 ml.) which was heated at 60° C. for 2 hours. Then, volatiles were removed under reduced pressure and the remaining mass was chromatographed on a column of silica gel with chloroform/acetone=85/15(V/V) to give 4.78 g of ethyl 5-fluoro-6-cyclobutylideneaminooxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate. Then, volatiles were removed under reduced pressure the remaining mass was chromatographed on a column of silica gel with chloroform/acetone=85/15(V/V)