HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 88600928, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3-Methylpyridine | HCID 7970 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 7-Aminocephalosporanic acid | HCID 441328 | — |
| Reactant | HCID 178427269 | HCID 178427269 | — |
| Solvent | Propan-2-ol--water (1/1) | HCID 21889133 | — |
| Product | HCID 88600928 | HCID 88600928 | 80% |
Reaction Steps
4.29 g (3 cmole) of 3-methylisoxazole-5-thiocarboxylic acid were dissolved in 300 ml of 60% isopropanol-water and there were added 1.6 ml of DBU (Example 9) and 3 ml of beta-picoline. At 65° C., there were added in one shot 3.0 g of 7-aminocephalosporanic acid, 90%. The mixture was stirred for 90 minutes and the reaction isoelectric pH was held to 5.5. The precipitate which formed was isolated after adjusting the pH to 4.0 at 25° C. by concentrated hydrochloric acid. The precipitate was filtered, washed with water and acetone to give 3.0 g of the compound of the title, with an 80% yield. The infrared and proton magnetic resonance spectra are consistent with its structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04481357 |
| Source dataset | uspto-grants-1984_11 |
| ORD ID | ord-cc859309d5604db3ab70ca80d59faac0 |
| Source note | uspto-grants-1984_11 |