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Methanol → 3-(Trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazine-7-carbaldehyde

HRID 1924327
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HRID 1924327 반응식
[CH3:1][C:2]1[CH:7]=[N:6][N:5]2[C:8]([C:11]([F:14])([F:13])[F:12])=[N:9][N:10]=[C:4]2[CH:3]=1.C[OH:16]>ClCCl>[F:13][C:11]([F:14])([F:12])[C:8]1[N:5]2[N:6]=[CH:7][C:2]([CH:1]=[O:16])=[CH:3][C:4]2=[N:10][N:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 887MethanolHCID 536292037-Methyl-3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine

생성물 1

HCID 536292043-(Trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazine-7-carbaldehyde수율 78%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A finely-ground powder of NaIO4 is added to a solution of 7-methyl-3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine x233 (0.52 g, 2.0 mmol) in absolute methanol (42 ml). The reaction mixture is stirred at room temperature for 1.5 h and diluted with an equal volume of dichloromethane. The mixture is filtered through the Celite layer, and the solvents are removed under reduced pressure. The residue (0.5 g) is purified by chromatography on silicagel (hexane/ethyl acetate 3/2) to yield 0.34 g of 3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazine-7-carbaldehyde x235 as a white solid.

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후처리

  1. filtrationThe mixture is filtered through the Celite layer
  2. customthe solvents are removed under reduced pressure
  3. customThe residue (0.5 g) is purified by chromatography on silicagel (hexane/ethyl acetate 3/2)

출처 및 근거

ORD 기록
ord-dbce2ce78cb446feb4aaf7e7d50a7187
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178533B2

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