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Potassium Phosphate, Tribasic → 6-Fluoro-4-nitrobiphenyl-3-carbonitrile

HRID 17531
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HRID 17531 반응식
Br[C:2]1[C:3]([F:13])=[CH:4][C:5]([N+:10]([O-:12])=[O:11])=[C:6]([CH:9]=1)[C:7]#[N:8].[C:14]1(B(O)O)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>O1CCCC1.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:13][C:3]1[C:2]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:9][C:6]([C:7]#[N:8])=[C:5]([N+:10]([O-:12])=[O:11])[CH:4]=1
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참가 물질

6

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 66827Phenylboronic AcidHCID 685846195-Bromo-4-fluoro-2-nitrobenzonitrile

생성물 1

HCID 685844646-Fluoro-4-nitrobiphenyl-3-carbonitrile

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매
HCID 8028
Tetrahydrofuran
용매

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온도
75 °C

실험 절차

5-Bromo-4-fluoro-2-nitrobenzonitrile (I-240) (9.1 g, 37.14 mmol) was dissolved in tetrahydrofuran (270 ml), and at room temperature, phenylboronic acid (9.06 g, 74.28 mmol), tripotassium phosphate (15.77 g, 74.28 mmol) and tetrakis(triphenylphosphine)palladium (2.15 g, 1.86 mmol) were added. After stirred under nitrogen atmosphere at 75° C. for 48 hours, this was cooled to room temperature. The insoluble matter was separated by filtration, the filtrate was concentrated under reduced pressure. The residue was fractionated with chloroform and aqueous saturated ammonium chloride solution. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate.

후처리

  1. temperaturethis was cooled to room temperature
  2. customThe insoluble matter was separated by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate

출처 및 근거

ORD 기록
ord-c16728b9ee0a48caa07a48e8b5a39f6b
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07737166B2

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