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Lithium hydroxide, monohydrate → 2-(3,5-Bis(trifluoromethyl)phenyl)-2-methylpropanoic acid

HRID 966970
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HRID 966970 반응식
O.[OH-].[Li+].[CH3:4][C:5]([CH3:24])([C:10]1[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[C:12]([C:20]([F:23])([F:22])[F:21])[CH:11]=1)[C:6]([O:8]C)=[O:7]>CO.O.O1CCCC1>[CH3:4][C:5]([CH3:24])([C:10]1[CH:11]=[C:12]([C:20]([F:21])([F:22])[F:23])[CH:13]=[C:14]([C:16]([F:17])([F:18])[F:19])[CH:15]=1)[C:6]([OH:8])=[O:7]
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참가 물질

6

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 219553242-(3,5-Bis-trifluoromethyl-phenyl)-2-methylpropionic acid, methyl ester

생성물 1

HCID 98359482-(3,5-Bis(trifluoromethyl)phenyl)-2-methylpropanoic acid수율 100%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

Lithium hydroxide monohydrate (2.13 g, 50.6 mmol) was added to a suspension of methyl α,α-dimethyl-3,5-bis(trifluoromethyl)benzeneacetate (Description 9, 5.3 g, 16.88 mmol) in methanol (60 mL), water (20 mL) and tetrahydrofuran (20 mL) and the mixture was degassed and stirred at room temperature for 3 days. The solvent was evaporated under reduced pressure and the residue was suspended in hydrochloric acid (1M). The mixture was extracted with ethyl acetate and the combined organic fractions were dried (MgSO4) and the solvent was evaporated under reduced pressure to give the title compound as a colorless solid (5.05 g, 100%). 1H NMR (400 MHz, CDCl3) δ 7.84 (2H, s), 7.80 (1H, s), and 1.68 (6H, s).

후처리

  1. customthe mixture was degassed
  2. customThe solvent was evaporated under reduced pressure
  3. extractionThe mixture was extracted with ethyl acetate
  4. dry with materialthe combined organic fractions were dried (MgSO4)
  5. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-db44576f04de402fa097391761b09bc2
출처 데이터셋
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06953792B2

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