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Water → 3'-Fluoro-4'-methylbiphenyl-2-carboxylic acid t-butyl ester

HRID 1810124
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HRID 1810124 반응식
[C:1]([O:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1Br)([CH3:4])([CH3:3])[CH3:2].[F:15][C:16]1[CH:17]=[C:18](B(O)O)[CH:19]=[CH:20][C:21]=1[CH3:22].C(O)(C)C.C(=O)([O-])[O-].[Na+].[Na+].O>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:1]([O:5][C:6]([C:7]1[C:8]([C:18]2[CH:19]=[CH:20][C:21]([CH3:22])=[C:16]([F:15])[CH:17]=2)=[CH:9][CH:10]=[CH:11][CH:12]=1)=[O:14])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

7

반응물 5

HCID 962WaterHCID 3776IsopropanolHCID 10340Sodium CarbonateHCID 27826743-Fluoro-4-methylbenzeneboronic acidHCID 3804415tert-Butyl 2-bromobenzoate

생성물 1

HCID 574839403'-Fluoro-4'-methylbiphenyl-2-carboxylic acid t-butyl ester수율 76.6%

시약·촉매·용매 1

HCID 178418397HCID 178418397, 화합물촉매

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온도
90 °C

실험 절차

Compound A (80.0 g, 311 mmol) and 3-fluoro-4-methylphenylboronic acid (52.7 g, 342 mmol) were suspended in isopropyl alcohol (260 mL, 3.5 mol). A solution of sodium carbonate (56.1 g, 529 mmol) in water (260 mL, 15 mol) was added and the mixture was degassed under nitrogen. Tetrakis(triphenylphosphine)palladium(0) (3.6 g, 3.1 mmol) was then added and the mixture was stirred at 90° C. for 17 hours. The mixture was concentrated under reduced pressure and suspended in water (200 mL). The aqueous phase was extracted with EtOAc (600 mL) and separated. The organic phase was washed with saturated aqueous NaCl and concentrated under reduced pressure. The recovered oil was purified by silica gel chromatography (4-6% 5×120 g column) to yield compound B as a clear oil (68.2 g).

후처리

  1. customthe mixture was degassed under nitrogen
  2. concentrationThe mixture was concentrated under reduced pressure
  3. extractionThe aqueous phase was extracted with EtOAc (600 mL)
  4. customseparated
  5. washThe organic phase was washed with saturated aqueous NaCl
  6. concentrationconcentrated under reduced pressure
  7. customThe recovered oil was purified by silica gel chromatography (4-6% 5×120 g column)

출처 및 근거

ORD 기록
ord-80623f272e7c479cb335546fb476ffbe
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362061B2

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