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Triacetoxyperiodinane → 1-(3-Methoxy-6-pyridin-4-yl-pyridazin-4-yl)-ethanone

HRID 1786687
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반응식

HRID 1786687 반응식
[CH3:1][O:2][C:3]1[N:4]=[N:5][C:6]([C:12]2[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=2)=[CH:7][C:8]=1[CH:9]([OH:11])[CH3:10].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C1=CC=CC=2)=O>C(Cl)Cl>[CH3:1][O:2][C:3]1[N:4]=[N:5][C:6]([C:12]2[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=2)=[CH:7][C:8]=1[C:9](=[O:11])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 159087TriacetoxyperiodinaneHCID 230925161-(3-Methoxy-6-pyridin-4-yl-pyridazin-4-yl)-ethanol

생성물 1

HCID 230924691-(3-Methoxy-6-pyridin-4-yl-pyridazin-4-yl)-ethanone수율 92%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 0.91 g 1-(3-methoxy-6-pyridin-4-yl-pyridazin-4-yl)-ethanol in 10 ml CH2Cl2 is added a suspension of 1.70 g Dess-Martin Periodane in 10 ml CH2Cl2 at room temperature. After being stirred for 3 h, the suspension is extracted with 5% aq. Na2S2O3 solution. The organic layer is washed with water, dried over MgSO4 and concentrated in vacuo. The residue is purified by chromatography to give 0.83 g (92%) of the desired product as a yellow solid.

후처리

  1. extractionthe suspension is extracted with 5% aq. Na2S2O3 solution
  2. washThe organic layer is washed with water
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by chromatography

출처 및 근거

ORD 기록
ord-fda2ba8339ae49b3950cb537d1f4f04f
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07507734B2

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