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Methanol → 5-[2-(3-methoxy-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamoyl]-1-methyl-1H-pyrazole-4-carboxylic acid

HRID 1802264
ノート
印刷プレビュー

反応式

HRID 1802264 の反応式
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH3:31])[C:10]=1[C:11](=[O:30])[NH:12][C:13]1[CH:18]=[CH:17][N:16]2[N:19]=[C:20]([C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([O:28][CH3:29])[CH:23]=3)[N:21]=[C:15]2[CH:14]=1)=[O:5])C.CO.O.[Li+].[OH-]>C1COCC1>[CH3:29][O:28][C:24]1[CH:23]=[C:22]([C:20]2[N:21]=[C:15]3[CH:14]=[C:13]([NH:12][C:11]([C:10]4[N:9]([CH3:31])[N:8]=[CH:7][C:6]=4[C:4]([OH:5])=[O:3])=[O:30])[CH:18]=[CH:17][N:16]3[N:19]=2)[CH:27]=[CH:26][CH:25]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 962Water2 回HCID 3939Lithium HydroxideHCID 677766035-[2-(3-methoxy-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamoyl]-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester

生成物 1

HCID 677739945-[2-(3-methoxy-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamoyl]-1-methyl-1H-pyrazole-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
25 °C

実験手順

To a solution of 5-[2-(3-methoxy-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamoyl]-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (3.5 g, 8.33 mmol) in a mixture of THF (20 ml), MeOH (14 ml) and water (7 ml) was added LiOH×H2O (1.0 g, 25.0 mmol) at 0° C. The reaction mixture was stirred at 25° C. for 4 h. Solvents were removed in vacuum and the resultant crude material was diluted with water (150 ml). The aqueous layer was washed with ether (2×100 ml), cooled to 0° C., and slowly acidified (pH 5) with aqueous 1N HCl solution under stirring. The resultant precipitated solid was filtered and dried under vacuum to give 5-[2-(3-methoxy-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamoyl]-1-methyl-1H-pyrazole-4-carboxylic acid as white solid (5.9 g; crude, quant). LC-MS: m/z=393.0 [M+H]+.

後処理

  1. customSolvents were removed in vacuum
  2. additionthe resultant crude material was diluted with water (150 ml)
  3. washThe aqueous layer was washed with ether (2×100 ml)
  4. temperaturecooled to 0° C.
  5. stirringunder stirring
  6. customThe resultant precipitated solid
  7. filtrationwas filtered
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-58abc3d56dc843409b7d922bbcb1f69f
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08349824B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート