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Lithium hydroxide, monohydrate → 2'-fluoro-5-(2-isopropyl-2H-pyrazol-3-yl)-4'-methyl-biphenyl-3-carboxylic acid

HRID 2091820
ノート
印刷プレビュー

反応式

HRID 2091820 の反応式
O[Li].O.C[O:5][C:6]([C:8]1[CH:9]=[C:10]([C:22]2[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][C:23]=2[F:29])[CH:11]=[C:12]([C:14]2[N:15]([CH:19]([CH3:21])[CH3:20])[N:16]=[CH:17][CH:18]=2)[CH:13]=1)=[O:7]>O.C1COCC1>[F:29][C:23]1[CH:24]=[C:25]([CH3:28])[CH:26]=[CH:27][C:22]=1[C:10]1[CH:11]=[C:12]([C:14]2[N:15]([CH:19]([CH3:21])[CH3:20])[N:16]=[CH:17][CH:18]=2)[CH:13]=[C:8]([C:6]([OH:7])=[O:5])[CH:9]=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 168937Lithium hydroxide, monohydrateHCID 577706482'-fluoro-5-(2-isopropyl-2H-pyrazol-3-yl)-4'-methyl-biphenyl-3-carboxylic acid methyl ester

生成物 1

HCID 577705982'-fluoro-5-(2-isopropyl-2H-pyrazol-3-yl)-4'-methyl-biphenyl-3-carboxylic acid収率 93%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of LiOH hydrate (82 mg, 1.94 mmol) in H2O (7 mL) was added dropwise to a solution of 2′-fluoro-5-(2-isopropyl-2H-pyrazol-3-yl)-4′-methyl-biphenyl-3-carboxylic acid methyl ester (524 mg, 1.49 mmol) in THF (4 mL) at 0° C. The reaction mixture was allowed to warm to room temperature and was stirred until the reaction solution turned into clear. Solvent was removed under vacuum and the resulting aqueous solution was acidified by 10% HCl to pH=6˜7. The resulting precipitate was collected and dried to afford 2′-fluoro-5-(2-isopropyl-2H-pyrazol-3-yl)-4′-methyl-biphenyl-3-carboxylic acid (468 mg, 93%).

後処理

  1. customSolvent was removed under vacuum
  2. customThe resulting precipitate was collected
  3. customdried

出典と根拠

ORDレコード
ord-654b0b3979fc4c908abf9c91c5a4efb6
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08440673B2

反応ノート

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