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Ethanol → 6-(4-Fluorophenyl)picolinic acid

HRID 15523
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HRID 15523 반응식
Br[C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][CH:3]=1.C([O-])([O-])=O.[Na+].[Na+].[F:17][C:18]1[CH:23]=[CH:22][C:21](B2OCC(C)(C)CO2)=[CH:20][CH:19]=1.CCO>COCCOC.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>[F:17][C:18]1[CH:23]=[CH:22][C:21]([C:2]2[N:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][CH:3]=2)=[CH:20][CH:19]=1
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7

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HCID 702EthanolHCID 10340Sodium CarbonateHCID 5939196-Bromopyridine-2-carboxylic acidHCID 110200772-(4-Fluorophenyl)-5,5-dimethyl-1,3,2-dioxaborinane

생성물 1

HCID 210817086-(4-Fluorophenyl)picolinic acid수율 46%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 80711,2-Dimethoxyethane용매

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온도
100 °C

실험 절차

A solution of 6-bromopicolinic acid (Aldrich) (2.02 g, 10 mmol) in DME containing 4 mL of 10% aq Na2CO3 was purged with Ar gas. To this mixture was added Pd(PPh3)4 followed by 2-(4-fluorophenyl)-5,5-dimethyl-1,3,2-dioxaborinane (2.40 g, 11.5 mmol, Wako Pure Chemical Industries, Ltd) and EtOH (20 mL), and the mixture was purged with Ar gas. The reaction mixture was heated at 100° C. for 2.5 h in a sealed tube. Additional 2-bromopicolinic acid (900 mg) and Pd (OAc)2 was added, and after purging with Ar gas it was heated at 100° C. for 4.5 h. Trifluoroacteic acid (20 mL) was added to the reaction mixture, concentrated and MeOH (150 mL) was added to the residue. The insoluble material was filtered, and the filtrate solution was concentrated. Purification by flash column on silica gel eluting with EtOAc/MeOH//900:100 followed by EtOAc/MeOH/HOAc//700:1500:50 provided the desired product (1.0 g, 40% based on borinane starting material) as a white solid. 1H NMR (CD3OD) δ 8.01 (d, 1H, J=7.7 Hz), 7.94-7.87 (m, 3H), 7.73 (d, 1H, J=7.7 Hz), 7.13 (t, 2H, 8.8 Hz); MS(ESI+) m/z 234 (M+H)+.

후처리

  1. customthe mixture was purged with Ar gas
  2. additionAdditional 2-bromopicolinic acid (900 mg) and Pd (OAc)2 was added
  3. customafter purging with Ar gas it
  4. temperaturewas heated at 100° C. for 4.5 h
  5. additionTrifluoroacteic acid (20 mL) was added to the reaction mixture
  6. concentrationconcentrated
  7. additionMeOH (150 mL) was added to the residue
  8. filtrationThe insoluble material was filtered
  9. concentrationthe filtrate solution was concentrated
  10. customPurification by flash column on silica gel eluting with EtOAc/MeOH//900:100

출처 및 근거

ORD 기록
ord-b3ac16c53b60473596afcd58d309504e
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07732613B2

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