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Water → HCID 69332723, 화합물

HRID 915036
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HRID 915036 반응식
[C:1]([C:3]1[C:4]([N:26]=CN(C)C)=[N:5][C:6]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)=[C:7]([C:9]2[CH:14]=[CH:13][C:12](=[O:15])[N:11]([CH:16]([CH3:18])[CH3:17])[N:10]=2)[N:8]=1)#[N:2].O.C([O-])(O)=O.[Na+].CCOC(C)=O>Cl.O1CCOCC1>[NH2:26][C:4]1[C:3]([C:1]#[N:2])=[N:8][C:7]([C:9]2[CH:14]=[CH:13][C:12](=[O:15])[N:11]([CH:16]([CH3:18])[CH3:17])[N:10]=2)=[C:6]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)[N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962Water2회HCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 69332615HCID 69332615, 화합물

생성물 1

HCID 69332723HCID 69332723, 화합물수율 69,432.602%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매
HCID 31275
1,4-Dioxane
용매

실험 절차

A solution of N′-[3-cyano-6-(4-fluorophenyl)-5-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-pyrazinyl]-N,N-dimethylimidoformamide (100 mg) in 4N HCl in dioxane (2 ml) and water (2 ml) was stirred at 25° C. for 15 hours. Water, aq. NaHCO3 and EtOAc were added to the reaction mixture. The organic layer was separated, and dried over MgSO4. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography eluted with a mixture of n-hexane and EtOAc. The fractions were concentrated in vacuo to obtain 3-amino-5-(4-fluorophenyl)-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-pyrazinecarbonitrile (60 g) as white powder.

후처리

  1. customThe organic layer was separated
  2. dry with materialdried over MgSO4
  3. customThe solvent was removed in vacuo
  4. customThe residue was purified by silica gel column chromatography
  5. washeluted with a mixture of n-hexane and EtOAc
  6. concentrationThe fractions were concentrated in vacuo

출처 및 근거

ORD 기록
ord-a61c7ecc0db74084b634ddc219fade7e
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07265120B2

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