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

HRID 928262

반응식

HRID 928262 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-9941235d6e0b4118a1762ec6c242905a
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290502B2

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