Potassium Persulfate → HCID 70390484, Verbindung

HRID 2231572Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2231572
[C:1]([NH:4][CH2:5][C@H:6]1[N:9](CC2C=CC(OC)=CC=2OC)[C:8](=[O:21])[C@H:7]1[NH:22][C:23](=[O:31])[CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)(=[O:3])[CH3:2].S(OOS([O-])(=O)=O)([O-])(=O)=O.[K+].[K+].P(O)([O-])([O-])=O.[K+].[K+]>O.C(#N)C>[C:1]([NH:4][CH2:5][C@H:6]1[NH:9][C:8](=[O:21])[C@H:7]1[NH:22][C:23](=[O:31])[CH2:24][C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1)(=[O:3])[CH3:2]

Komponenten

6

Edukt 3

HCID 24412Potassium PersulfateHCID 24450Potassium Phosphate, DibasicHCID 70390712HCID 70390712, Verbindung

Produkt 1

HCID 70390484HCID 70390484, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 298 mg of cis-4-acetamidomethyl-1-(2,4-dimethoxybenzyl)-3-phenylacetamido-2-oxoazetidine, 576 mg of potassium persulfate and 183 mg of dipotassium phosphate in 15 ml of water and 15 ml of acetonitrile is heated under reflux for 1.5 hours. The reaction mixture is concentrated in vacuo. The residue is taken up in ethyl acetate and the solution is washed successively with an aqueous sodium hydrogen carbonate solution and an aqueous sodium chloride solution. The ethyl acetate solution is dried over magnesium sulfate and the solvent is then distilled off in vacuo. Ethyl acetate is added to the residue and the precipitated crystals are collected by filtration to give cis-4-acetamidomethyl-3-phenylacetamido-2-oxoazetidine, m.p. 200°-202° C.

Aufarbeitung

  1. temperatureis heated
  2. temperatureunder reflux for 1.5 hours
  3. concentrationThe reaction mixture is concentrated in vacuo
  4. washthe solution is washed successively with an aqueous sodium hydrogen carbonate solution
  5. dry with materialThe ethyl acetate solution is dried over magnesium sulfate
  6. distillationthe solvent is then distilled off in vacuo
  7. additionEthyl acetate is added to the residue
  8. filtrationthe precipitated crystals are collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-4c72b50d78c14712b22ff5243a8273bf
Quelldatensatz
uspto-grants-1988_11
Patentnummer
US04782147

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