反应详情

To a solution of 325 mg. (0.7 mmole) of p-nitrobenzyl 7-[2-(2-thienyl)acetamido]-3-hydroxy-3-cephem-4-carboxylate in 10 ml. of methylene chloride was slowly added an equivalent amount of N-(2-chloro-1,1,2-trifluoroethyl) diethylamine. The reaction mixture was heated for 30 minutes under gentle reflux and was then evaporated to dryness in vacuo. The residue was dissolved in a mixture of ethyl acetate-water and the organic layer was separated. The organic layer was washed with 5% hydrochloric acid, water and brine and was then dried. The dried reaction product solution was concentrated to a small volume and n-hexane was added to precipitate, p-nitrobenzyl 7-[2-(2-thienyl)acetamido]-3-fluoro-3-cephem-4-carboxylate.

1. temperatureThe reaction mixture was heated for 30 minutes
2. temperatureunder gentle reflux
3. customwas then evaporated to dryness in vacuo
4. dissolutionThe residue was dissolved in a mixture of ethyl acetate-water
5. customthe organic layer was separated
6. washThe organic layer was washed with 5% hydrochloric acid, water and brine
7. customwas then dried
8. customThe dried reaction product solution
9. concentrationwas concentrated to a small volume and n-hexane
10. additionwas added
11. customto precipitate