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1,1'-(Diazomethylene)bis(benzene) → HCID 88777142, 화합물

HRID 1657422
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HRID 1657422 반응식
[C:1]1([C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[N+]=[N-])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:16]([C:18]1[CH:23]([C:24]([OH:26])=[O:25])[N:22]2[C:27](=[O:38])[CH:28]([NH:29][C:30](=[O:37])[CH2:31][C:32]3[S:33][CH:34]=[CH:35][CH:36]=3)[C@H:21]2[S:20][CH:19]=1)=[O:17]>O1CCCC1>[CH:16]([C:18]1[CH:23]([C:24]([O:26][CH:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[O:25])[N:22]2[C:27](=[O:38])[CH:28]([NH:29][C:30](=[O:37])[CH2:31][C:32]3[S:33][CH:34]=[CH:35][CH:36]=3)[C@H:21]2[S:20][CH:19]=1)=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 612301,1'-(Diazomethylene)bis(benzene)HCID 88777331HCID 88777331, 화합물

생성물 1

HCID 88777142HCID 88777142, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of diphenyldiazomethane (0.213 g, 1.1 mmol) in dry tetrahydrofuran (2 ml) was added dropwise with stirring to the 3-formyl-7-(2-thienylacetamido)-2-cephem-4-carboxylic acid (0.352 g., 1 mmol) in dry tetrahydrofuran (10 ml) at 40°. The reagent was allowed to completely react as noted by the color changes between each addition. The reaction was stirred at 40° for 2 hours after the addition was completed and then the solvent was removed in vacuo. The residual oil was dissolved in chloroform, washed with 5% NaHCO3, dried over MgSO4 and concentrated to half volume. The product was precipitated by the addition of hexane.

후처리

  1. customto completely react
  2. additionas noted by the color changes between each addition
  3. additionafter the addition
  4. customthe solvent was removed in vacuo
  5. dissolutionThe residual oil was dissolved in chloroform
  6. washwashed with 5% NaHCO3
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated to half volume
  9. customThe product was precipitated by the addition of hexane

출처 및 근거

ORD 기록
ord-c88c869255de4afb8521078d21ad9050
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03960852

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