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4-(Trifluoromethyl)phenylboronic acid → 2,6-Dimethyl-4-nitro-4'-(trifluoromethyl)biphenyl

HRID 2173797
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HRID 2173797 반응식
Br[C:2]1[C:7]([CH3:8])=[CH:6][C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[CH3:12].[F:13][C:14]([F:25])([F:24])[C:15]1[CH:20]=[CH:19][C:18](B(O)O)=[CH:17][CH:16]=1.O.[F-].[K+]>C1(C)C=CC=CC=1.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>[CH3:12][C:3]1[CH:4]=[C:5]([N+:9]([O-:11])=[O:10])[CH:6]=[C:7]([CH3:8])[C:2]=1[C:18]1[CH:19]=[CH:20][C:15]([C:14]([F:25])([F:24])[F:13])=[CH:16][CH:17]=1
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참가 물질

6

반응물 3

HCID 27343894-(Trifluoromethyl)phenylboronic acidHCID 70220962-Bromo-1,3-dimethyl-5-nitrobenzeneHCID 23675105Potassium fluoride hydrate

생성물 1

HCID 674856592,6-Dimethyl-4-nitro-4'-(trifluoromethyl)biphenyl수율 43.4%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매
HCID 1140Toluene용매

실험 절차

To a solution of 2-bromo-1,3-dimethyl-5-nitrobenzene (2.7 g, 11.7 mmol) in toluene (36 mL) was added tetrakis(triphenylphosphine)palladium(0) (1.36 g, 1.17 mmol), 4-(trifluoromethyl)phenylboronic acid (4.46 g, 23.5 mmol), and potassium fluoride hydrate (3.31 g, 43 mmol). The reaction was purged with nitrogen three times. Water (9 mL) was added and the reaction was refluxed overnight. The reaction was diluted with saturated ammonium chloride and the layers were separated. The organic layer was washed with water (3×40 mL) and brine, dried over sodium sulfate, filtered and concentrated. Purification by column chromatography gave 2,6-dimethyl-4-nitro-4′-(trifluoromethyl)biphenyl (1.5 g, 43%) as a yellow solid. 1H NMR (400 MHz, CDCl3, δ): 7.99 (s, 2H), 7.75 (d, 2H), 7.26 (s, 1H), 7.25 (s, 1H), 2.10 (s, 6H).

후처리

  1. customThe reaction was purged with nitrogen three times
  2. additionWater (9 mL) was added
  3. temperaturethe reaction was refluxed overnight
  4. additionThe reaction was diluted with saturated ammonium chloride
  5. customthe layers were separated
  6. washThe organic layer was washed with water (3×40 mL) and brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customPurification by column chromatography

출처 및 근거

ORD 기록
ord-58cee13e4f6843d287259b3071ce736e
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056834B2

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