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Lithium Hydroxide → 5-Bromo-6-(4-fluoro-phenyl)-pyrazine-2-carboxylic acid

HRID 1865876
ノート
印刷プレビュー

反応式

HRID 1865876 の反応式
C[O:2][C:3]([C:5]1[CH:10]=[N:9][C:8]([Br:11])=[C:7]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[N:6]=1)=[O:4].[OH-].[Li+]>O1CCCC1.O>[Br:11][C:8]1[N:9]=[CH:10][C:5]([C:3]([OH:4])=[O:2])=[N:6][C:7]=1[C:12]1[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 866169575-Bromo-6-(4-fluoro-phenyl)-pyrazine-2-carboxylic acid methyl ester

生成物 1

HCID 866169585-Bromo-6-(4-fluoro-phenyl)-pyrazine-2-carboxylic acid収率 100.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 0.81 g 5-bromo-6-(4-fluoro-phenyl)-pyrazine-2-carboxylic acid methyl ester in 10 ml tetrahydrofuran was added at room temperature 2.6 ml of a 1M solution of lithium hydroxide in water and the mixture was stirred for 15 minutes. The resulting solution was partitioned between 10% aqueous citric acid and ethyl acetate. The phases were separated and the organic layer washed with water and brine. The organic phase was dried over magnesium sulfate and evaporated to yield 0.78 g of the title compound as white crystals. MS (ISP) (M+H+)=297.2 and 299.0.

後処理

  1. customThe resulting solution was partitioned between 10% aqueous citric acid and ethyl acetate
  2. customThe phases were separated
  3. washthe organic layer washed with water and brine
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. customevaporated

出典と根拠

ORDレコード
ord-fed9016c8f11439eb9a9384bac4b16da
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07629346B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート