Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methylthioacetyl chloride | HCID 21249692 | — |
| Reactant | HCID 178468135 | HCID 178468135 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 178468134 | HCID 178468134 | — |
Reaction Steps
To a stirred, cooled (-20°) solution of 11.34 g (0.026 mol) of 7-amino-3-(1-ethoxyhydroxyphosphinylmethyltetrazol-5-ylthiomethyl)-3-cephem-4-carboxylic acid in 220 ml of 3% sodium bicarbonate and 220 ml of acetone is added dropwise a solution of 3.66 g (0.029 mol) of methylthioacetyl chloride in 52 ml of acetone, during which time the pH of the reaction mixture is maintained at 8.0 by addition of 10% sodium hydroxide. After addition the reaction mixture is stirred an additional 20 minutes at -15°, then is warmed to 25° and extracted with ether. The aqueous phase is passed down a XAD-7 resin column and the product-containing fractions are combined, treated with Amberlite IR-120H ion-exchange resin and lyophilized to yield the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04112086 |
|---|
| Source dataset | uspto-grants-1978_09 |
|---|
| ORD ID | ord-9ab5913d20c64a3499b97a99ea1fd1f6 |
|---|
| Source note | uspto-grants-1978_09 |
|---|