Potassium Persulfate → HCID 70390484, 화합물

HRID 653292노트

반응식

HRID 653292 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 70390484HCID 70390484, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8277827553d346229226ec46ab1f836d
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04675397

반응 노트

불러오는 중…