Lithium hydroxide, monohydrate → 5-[3-(4-Fluoro-phenyl)-5-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyrazine-2-carboxylic acid

HRID 402456ノート

反応式

HRID 402456 の反応式
O.[OH-].[Li+].C[O:5][C:6]([C:8]1[CH:13]=[N:12][C:11]([O:14][CH2:15][C:16]2[N:17]([C:22]3[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=3)[N:18]=[N:19][C:20]=2[CH3:21])=[CH:10][N:9]=1)=[O:7]>O.C1COCC1>[F:28][C:25]1[CH:24]=[CH:23][C:22]([N:17]2[C:16]([CH2:15][O:14][C:11]3[N:12]=[CH:13][C:8]([C:6]([OH:7])=[O:5])=[N:9][CH:10]=3)=[C:20]([CH3:21])[N:19]=[N:18]2)=[CH:27][CH:26]=1

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 674980315-[3-(4-fluoro-phenyl)-5-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester

生成物 1

HCID 674987585-[3-(4-Fluoro-phenyl)-5-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyrazine-2-carboxylic acid収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of lithium hydroxide monohydrate (180 mg, 4.25 mmol) in water (7.3 mL) was added dropwise to a suspension of 5-[3-(4-fluoro-phenyl)-5-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester (730 mg, 2.13 mmol) in THF (7.3 mL). The reaction mixture was then stirred at room temperature for 30 min and was then evaporated and the residue dissolved in water, acidified with HCl (1N), and the resulting precipitate filtered off to afford the title product (700 mg, 100%) as a white solid. MS: m/e=330.1 [M−H]−.

後処理

  1. customwas then evaporated
  2. dissolutionthe residue dissolved in water
  3. filtrationthe resulting precipitate filtered off

出典と根拠

ORDレコード
ord-35dc9735a7f24ebe9153ea890e7c7cef
出典データセット
uspto-grants-2014_06
特許番号
US08742097B2

反応ノート

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