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Potassium Carbonate → 2-(4-chlorophenyl)-5-nitropyridine

HRID 881758
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인쇄 미리보기

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HRID 881758 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[Cl:11][C:12]1[CH:17]=[CH:16][C:15](B(O)O)=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+].O1CCOCC1>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.O>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=2)=[CH:14][CH:13]=1
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참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 742994-Chlorophenylboronic acidHCID 782402-Bromo-5-nitropyridine

생성물 1

HCID 27638652-(4-chlorophenyl)-5-nitropyridine수율 103.8%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 962Water용매

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온도
100 °C

실험 절차

A flask was charged with 2-bromo-5-nitropyridine (4 g, 19.71 mmol), 4-chlorophenylboronic acid (4.54 g, 27.6 mmol), Pd(PPh3)4 (1.139 g, 0.985 mmol), potassium carbonate (8.16 g, 59.1 mmol), dioxane (40 ml) and water (20 ml) at room temperature. The flask was sealed, flushed with nitrogen for three times and heated at 100° C. for 3 hours. The reaction mixture was diluted with EtOAc (100 ml) and filtered. The filtrate was concentrated. The residue was washed with water by filtration. The afforded solid was dissolved in EtOAc (200 ml) and washed with saturated aqueous sodium bicarbonate solution and brine, dried over Na2SO4, concentrated, and dried under vacuum to afford crude 2-(4-chlorophenyl)-5-nitropyridine (4.8 g, 75% purity, 78% yield) as yellow solid. 1H NMR (400 MHz, DMSO-d6) ppm 7.27-7.36 (m, 4H) 7.51-7.61 (m, 3H).

후처리

  1. customThe flask was sealed
  2. customflushed with nitrogen for three times
  3. additionThe reaction mixture was diluted with EtOAc (100 ml)
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated
  6. washThe residue was washed with water by filtration
  7. dissolutionThe afforded solid was dissolved in EtOAc (200 ml)
  8. washwashed with saturated aqueous sodium bicarbonate solution and brine
  9. dry with materialdried over Na2SO4
  10. concentrationconcentrated
  11. customdried under vacuum

출처 및 근거

ORD 기록
ord-f462997f79f64c07b3aa1a5a22c5e1d5
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08993619B2

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