HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Chloride → HCID 131712941, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | HCID 140338070 | HCID 140338070 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 131712941 | HCID 131712941 | 53.9% |
Reaction Steps
In tetrahydrofuran (20 ml) is dissolved 2,2,2-trichloroethyl (E)-7-t-butoxycarbonylhydrazono-3-methyl-3-cephem-4-carboxylate (4.60 g), and under ice-cooling, a 1 M tetrahydrofuran solution of borane-tetrahydrofuran complex (23 ml) is added dropwise. The mixture is stirred at that temperature for 30 minutes. The reaction mixture is poured in a mixture of ethyl acetate (150 ml) and aqueous sodium chloride (200 ml). The organic layer is taken, dried over magnesium sulfate and concentrated. The residual oil is subjected to silica gel (50 g) column chromatography and elution is carried out with ethyl acetate-benzene. The above procedure gives crystals of 2,2,2-trichloroethyl 7β-t-butoxycarbonylhydrazino-3-methyl-3-cephem-4-carboxylate (2.49 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04369312 |
| Source dataset | uspto-grants-1983_01 |
| ORD ID | ord-0e31274a0c71416ebc1038af4996cc15 |
| Source note | uspto-grants-1983_01 |