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Lithium Hydroxide → 1-({5-[3-(trifluoromethyl)phenyl]-1,2,4-oxadiazol-3-yl}methyl)-1H-pyrazole-4-carboxylic acid

HRID 1257418
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HRID 1257418 반응식
[F:1][C:2]([F:26])([F:25])[C:3]1[CH:4]=[C:5]([C:9]2[O:13][N:12]=[C:11]([CH2:14][N:15]3[CH:19]=[C:18]([C:20]([O:22]CC)=[O:21])[CH:17]=[N:16]3)[N:10]=2)[CH:6]=[CH:7][CH:8]=1.[OH-].[Li+]>C(O)C.O>[F:26][C:2]([F:1])([F:25])[C:3]1[CH:4]=[C:5]([C:9]2[O:13][N:12]=[C:11]([CH2:14][N:15]3[CH:19]=[C:18]([C:20]([OH:22])=[O:21])[CH:17]=[N:16]3)[N:10]=2)[CH:6]=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 66939395ethyl 1-({5-[3-(trifluoromethyl)phenyl]-1,2,4-oxadiazol-3-yl}methyl)-1H-pyrazole-4-carboxylate

생성물 1

HCID 669395711-({5-[3-(trifluoromethyl)phenyl]-1,2,4-oxadiazol-3-yl}methyl)-1H-pyrazole-4-carboxylic acid수율 28%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

The compound (0.85 g) obtained in Example 114b was dissolved in ethanol (8 mL) and water (2 ml), and lithium hydroxide (0.42 g) was added. The reaction mixture was stirred at room temperature overnight and concentrated under reduced pressure. The residue was diluted with water and adjusted to pH 5-6 with 1N hydrochloric acid. The resulting precipitate was collected by filtration and the obtained solid was recrystallized from ethyl acetate-petroleum ether to give the title compound (0.22 g) as a colorless solid.

후처리

  1. concentrationconcentrated under reduced pressure
  2. additionThe residue was diluted with water
  3. filtrationThe resulting precipitate was collected by filtration
  4. customthe obtained solid was recrystallized from ethyl acetate-petroleum ether

출처 및 근거

ORD 기록
ord-fcd64fa794aa45dcaad9cfad75e534d0
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461348B2

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