反应详情

Acetic acid (4.5 ml) and zinc powder (3.6 g) were added under stirring and ice-cooling to a solution of 2,2,2-trichloroethyl 2-methyl-7-(2-phenylthioacetamido)-3-cephem-4-carboxylate (2.79 g) in anhydrous dimethylformamide (15 ml), and the mixture was stirred for 2 hours at the same temperature. After the reaction, zinc powder was filtered off, and the filtrate was poured into a mixture of 5% hydrochloric acid (75 ml) and ethyl acetate (50 ml), and extracted. The extract was washed with water and dried. After the solvent was distilled off, the residue was crystalized by adding ether to give colorless crystals of 2-methyl-7-(2-phenylthioacetamido)-3-cephem-4-carboxylic acid (2.0 g), mp 168° to 171° C. (dec.).

1. stirringthe mixture was stirred for 2 hours at the same temperature
2. filtrationwas filtered off
3. additionthe filtrate was poured into a mixture of 5% hydrochloric acid (75 ml) and ethyl acetate (50 ml)
4. extractionextracted
5. washThe extract was washed with water
6. customdried
7. distillationAfter the solvent was distilled off
8. customthe residue was crystalized
9. additionby adding ether