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Water → HCID 69332723、化合物

HRID 915036
ノート
印刷プレビュー

反応式

HRID 915036 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962Water2 回HCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 69332615HCID 69332615、化合物

生成物 1

HCID 69332723HCID 69332723、化合物収率 69,432.602%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒
HCID 31275
1,4-Dioxane
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a61c7ecc0db74084b634ddc219fade7e
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07265120B2

反応ノート

読み込み中…

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