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

HRID 2091820
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HRID 2091820 반응식
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
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 577706482'-fluoro-5-(2-isopropyl-2H-pyrazol-3-yl)-4'-methyl-biphenyl-3-carboxylic acid methyl ester

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-654b0b3979fc4c908abf9c91c5a4efb6
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08440673B2

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