HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 2-Methyl-7-(2-phenylthioacetamido)-3-cephem-4-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 2,2,2-Trichloroethyl 2-methyl-7-(2-phenylthioacetamido)-3-cephem-4-carboxylate | HCID 131711252 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-Methyl-7-(2-phenylthioacetamido)-3-cephem-4-carboxylic acid | HCID 131711255 | 98.7% |
Reaction Steps
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.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04308380 |
| Source dataset | uspto-grants-1981_12 |
| ORD ID | ord-1a1cb888542f46398dabb042e6909aae |
| Source note | uspto-grants-1981_12 |