Sodium Iodide → HCID 70391052, 화합물

HRID 621031노트

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HRID 621031 반응식
[CH3:1][O:2][C:3]1[CH:36]=[C:35]([O:37][CH3:38])[CH:34]=[CH:33][C:4]=1[CH2:5][N:6]1[C@H:9]([CH2:10]OS(C2C=CC(C)=CC=2)(=O)=O)[C@H:8]([NH:22][C:23](=[O:31])[CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:7]1=[O:32].[I-:39].[Na+]>CC(C)=O>[CH3:1][O:2][C:3]1[CH:36]=[C:35]([O:37][CH3:38])[CH:34]=[CH:33][C:4]=1[CH2:5][N:6]1[C@H:9]([CH2:10][I:39])[C@H:8]([NH:22][C:23](=[O:31])[CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:7]1=[O:32]

참가 물질

4

반응물 2

HCID 5238Sodium IodideHCID 86740463HCID 86740463, 화합물

생성물 1

HCID 70391052HCID 70391052, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To 70 ml of acetone was added 2.27 g of cis-1-(2,4-dimethoxybenzyl)-3-phenylacetamido-4-(p-toluenesulfonyloxymethyl)-2-oxoazetidine and 4.95 g of sodium iodide, and the mixture is heated under reflux for 6 hours with stirring, and then concentrated in vacuo. To the residue are added methylene chloride and water to dissolve it, and the methylene chloride layer is separated and washed successively with an aqueous sodium thiosulfate solution and an aqueous sodium chloride solution. The methylene chloride layer is then dried over magnesium sulfate and the solvent is distilled off in vacuo. Ethyl acetate is added to the residue and the precipitated crystals are collected by filtration to give cis-1-(2,4-dimethoxybenzyl)-4-iodomethyl-3-phenylacetamido-2-oxoazetidine, m.p. 181°-182° C.

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 6 hours
  3. concentrationconcentrated in vacuo
  4. additionTo the residue are added methylene chloride and water
  5. dissolutionto dissolve it
  6. customthe methylene chloride layer is separated
  7. washwashed successively with an aqueous sodium thiosulfate solution
  8. dry with materialThe methylene chloride layer is then dried over magnesium sulfate
  9. distillationthe solvent is distilled off in vacuo
  10. additionEthyl acetate is added to the residue
  11. filtrationthe precipitated crystals are collected by filtration

출처 및 근거

ORD 기록
ord-75a0f7f8f86a49a1b7d00d1246224293
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04822790

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