Water → 6-(6-amino-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone

HRID 915038ノート

反応式

HRID 915038 の反応式
[CH:1]([N:4]1[C:9](=[O:10])[CH:8]=[CH:7][C:6]([C:11](=O)[C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=O)=[N:5]1)([CH3:3])[CH3:2].Br.Br.[NH2:23][CH2:24][C:25]([NH2:27])=[NH:26].C[O-].[Na+].O>CO.CCOC(C)=O>[NH2:27][C:25]1[N:26]=[C:11]([C:6]2[CH:7]=[CH:8][C:9](=[O:10])[N:4]([CH:1]([CH3:3])[CH3:2])[N:5]=2)[C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[N:23][CH:24]=1

参加物

7

反応物 4

HCID 962WaterHCID 10942334Sodium MethoxideHCID 16211382Aminoacetamidine DihydrobromideHCID 46832460HCID 46832460、化合物

生成物 1

HCID 693314606-(6-amino-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone収率 7.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 1-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-phenyl-1,2-ethanedione (300 mg), aminoacetamidine dihydrobromide (259 mg) and sodium methoxide (238 mg) in MeOH (3 ml) was stirred for 1.5 hours. Water 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 6-(6-amino-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone (25.6 mg) 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-2f96f97846c44ad391fbe7945cf43dcb
出典データセット
uspto-grants-2007_09
特許番号
US07265120B2

反応ノート

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