Potassium Persulfate → HCID 70390484、化合物

HRID 621126ノート

反応式

HRID 621126 の反応式
[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]

参加物

6

反応物 3

HCID 24412Potassium PersulfateHCID 24450Potassium Phosphate, DibasicHCID 70390712HCID 70390712、化合物

生成物 1

HCID 70390484HCID 70390484、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-310e56d019e64de981114a230cbac7e6
出典データセット
uspto-grants-1989_04
特許番号
US04822788

反応ノート

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