HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl carbazate → HCID 140338070, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl carbazate | HCID 70091 | — |
| Reactant | Pyridinium chloride | HCID 10176127 | — |
| Reactant | HCID 70464109 | HCID 70464109 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 140338070 | HCID 140338070 | 25.6% |
Reaction Steps
In chloroform (70 ml) are dissolved 2,2,2-trichloroethyl 3-methyl-7-oxo-3-cephem-4-carboxylate (14.30 g), t-butyl carbazate (6.00 g) and pyridine hydrochloride (4.77 g) and the mixture is refluxed in a Dean-Stark trap packed with Molecular Sieve 3A for 30 minutes. The reaction mixture is washed with 1 N-HCl and water in that order, dried over magnesium sulfate and concentrated. The residual oil is subjected to silica gel (240 g) column chromatography and elution is carried out with ethyl acetate-benzene to give crystals of 2,2,2-trichloroethyl (E)-7-t-butoxycarbonylhydrazono-3-methyl-3-cephem-4-carboxylate (4.88 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04369312 |
| Source dataset | uspto-grants-1983_01 |
| ORD ID | ord-c86c08d664ec46f1a49108fa893f1303 |
| Source note | uspto-grants-1983_01 |