反应详情

4.44 g of diphosphorus tetraiodide were suspended in 35 ml of pyridine, and after stirring for 5 minutes, 3.058 g of 1,1-dimethylethyl 7-[2-(2-tritylaminothiazol-4-yl)-2-methoxyimino-acetamido]-8-oxo-2-hydroxy-3-methoxymethyl-4-thia-1-azabicyclo[4,2,0]octane-2-carboxylate were added all at once with stirring for 2 hours 40 minutes. The pyridine was distilled off and the residue was taken up in 50 ml of ethyl acetate. After filtering, 50 ml of N hydrochloric acid were added to the filtrate with vigorous stirring and the decanted organic phase was washed with water, dried and concentrated to dryness under reduced pressure. The residue was chromatographed over silica and eluted with a mixture of methylene chloride and ethyl acetate (85-15). The fractions of interest were concentrated to dryness and crystallized from methanol to obtain 703 mg of 1,1-dimethylethyl 7-[2-(2-tritylaminothiazol-4-yl)-2-methoxyimino-acetamido]-8-oxo-3-methoxymethyl-4-thia-1-azabicyclo[4,2,0]oct-2-en-2-carboxylate

1. stirringwith stirring for 2 hours 40 minutes
2. distillationThe pyridine was distilled off
3. filtrationAfter filtering
4. addition50 ml of N hydrochloric acid were added to the filtrate
5. stirringwith vigorous stirring
6. washthe decanted organic phase was washed with water
7. customdried
8. concentrationconcentrated to dryness under reduced pressure
9. customThe residue was chromatographed over silica
10. washeluted with a mixture of methylene chloride and ethyl acetate (85-15)
11. concentrationThe fractions of interest were concentrated to dryness
12. customcrystallized from methanol