HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → HCID 67658279, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | HCID 67657400 | HCID 67657400 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 67658279 | HCID 67658279 | 5.6% |
Reaction Steps
A mixture of t-butyl 7α-bromo-3-methyl-3-cephem -4-carboxylate 1,1-dioxide (700 mg, 1.9 mmol), dimethylamine hydrochloride (460 mg, 5.7 mmol), methylene chloride (3 ml) and t-butyl alcohol (50 ml), formaldehyde (0.57 g, 37% w/v) was heated to reflux at 80°-90° C. for 20 hours. t-Butyl alcohol was removed under reduced pressure and the residue was dissolved in methylene chloride, washed with water, brine, dried and concentrated to give 200 mg of crude product which was purified over silica column using methylene chloride as eluant to give 40 mg of pure t-butyl 7α-bromo-2-methylene-3-methyl-3-cephem-4-carboxylate 1,1-dioxide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05264429 |
| Source dataset | uspto-grants-1993_11 |
| ORD ID | ord-1d812d9e7d0440fcb680da2e92c818d1 |
| Source note | uspto-grants-1993_11 |