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Lithium hydroxide, monohydrate → 2-[3-(trifluoromethyl)-1H-pyrazol-1-yl]acetic acid

HRID 1753076
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HRID 1753076 반응식
O.[OH-].[Li+].C([O:6][C:7](=[O:18])[CH2:8][N:9]1[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[N:10]1)C>O.C1COCC1>[F:17][C:14]([F:15])([F:16])[C:11]1[CH:12]=[CH:13][N:9]([CH2:8][C:7]([OH:18])=[O:6])[N:10]=1
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 2064143Ethyl 2-(3-(trifluoromethyl)-1H-pyrazol-1-yl)acetate

생성물 1

HCID 20608832-[3-(trifluoromethyl)-1H-pyrazol-1-yl]acetic acid수율 19.2%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Lithium hydroxide monohydrate (127 mg, 3.03 mmol) in water (0.5 mL) was added to (3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid ethyl ester (250 mg, 1.125 mmol) in THF (5 mL). The mixture was stirred at room temperature for 5 hours then the reaction mixture volume was reduced to one third by evaporation in vacuo. The aqueous residue was acidified using aqueous HCl (2M) to pH=5. The resulting off white solid was filtered, collected and dried, washed with ether to afford the title compound as a white solid (42 mg, 19%).

후처리

  1. customthe reaction mixture volume was reduced to one third by evaporation in vacuo
  2. filtrationThe resulting off white solid was filtered
  3. customcollected
  4. customdried
  5. washwashed with ether

출처 및 근거

ORD 기록
ord-9d52e78fb76b4841946e366f86da170a
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09163021B2

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