Acetic Acid → 2-(5-Bromo-2-fluoro-phenyl)-3H-pteridin-4-one

HRID 928262

反応式

HRID 928262 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:20])=[C:6]([CH:19]=1)[C:7]([NH:9][C:10]1[C:11]([C:16]([NH2:18])=[O:17])=[N:12][CH:13]=[CH:14][N:15]=1)=O.[OH-].[K+].CC(O)=O>O.CS(C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:20])=[C:6]([C:7]2[NH:18][C:16](=[O:17])[C:11]3[C:10](=[N:15][CH:14]=[CH:13][N:12]=3)[N:9]=2)[CH:19]=1

参加物

6

反応物 3

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 577423843-(5-Bromo-2-fluorobenzoylamino)pyrazine-2-carboxamide

生成物 1

HCID 1361099582-(5-Bromo-2-fluoro-phenyl)-3H-pteridin-4-one収率 84.1%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

A mixture of 3-(5-bromo-2-fluorobenzoylamino)pyrazine-2-carboxamide 103 (2.3 g, 6.78 mmol) and KOH (3.81 g, 67.8 mmol) in H2O (60 mL) and DMSO (20 mL) was stirred at room temperature for 45 min. Acidification to pH 5 (pH paper control) with AcOH followed by addition of 50 mL of ice-cold water afforded a precipitate, which was filtered off, washed with H2O, acetonitrile and ether to give 1.83 g of the title product 104 as a white powder (LCMS analysis).

後処理

  1. customafforded a precipitate, which
  2. filtrationwas filtered off
  3. washwashed with H2O, acetonitrile and ether

出典と根拠

ORDレコード
ord-9941235d6e0b4118a1762ec6c242905a
出典データセット
uspto-grants-2016_03
特許番号
US09290502B2

関連ノート

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