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Potassium Carbonate → HCID 10308060, 화합물

HRID 2099501
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HRID 2099501 반응식
Br[C:2]1[CH:3]=[N:4][N:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=2)[CH:6]=1.[C:13]([C:15]1[CH:16]=[C:17](B(O)O)[CH:18]=[CH:19][CH:20]=1)#[N:14].C(=O)([O-])[O-].[K+].[K+]>COCCOC.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>[N:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[N:5]1[CH:6]=[C:2]([C:19]2[CH:20]=[C:15]([CH:16]=[CH:17][CH:18]=2)[C:13]#[N:14])[CH:3]=[N:4]1
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참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 27343253-Cyanophenylboronic acidHCID 113451062-(4-bromo-1h-pyrazol-1-yl)pyridine

생성물 1

HCID 10308060HCID 10308060, 화합물

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매HCID 962Water
용매
HCID 80711,2-Dimethoxyethane용매

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온도
70 °C

실험 절차

A solution of 2-(4bromo-1H-pyrazol-1-yl)pyridine (0.446 g, 2.0 mmol), 3-cyanophenylboronic acid (0.302 g, 2.0 mmol), potassium carbonate (0.552 g, 4.0 mmol) in a mixture of ethylene glycol dimethyl ether (20 mL) and water (4 mL) was degassed by argon bubbling for 15 min., then tetrakis(triphenylphosphine)palladium(0) (20 mg, 0.017 mmol) was added and degassing continued a further 15 min. The resulting solution was stirred at 70° C. for 14 h, whereupon H2O (30 mL) was added, then extracted with EtOAc (3×30 mL) and the combined extracts washed with brine. The organic phase was dried over Na2SO4 and concentrated in vacuo. The crude residue was chromatographed on silica gel eluting with EtOAc:hexane (2:3) to afford a white solid which was recrystallized from EtOAc/Hexane give 3-(1-pyridin-2-yl-1H-pyrazol-4-yl)benzonitrile as a white solid. MP=160-161° C. 1H NMR (CD3Cl, 300 MHz) δ 8.88 (s, 1H), 8.45 (d, 1H), 8.03 (s, 1H), 8.01 (d, 1H), 7.87 (d, 1H), 7.86 (s, 1H), 7.81 (d, 1H), 7.57˜7.48 (m, 2H), 7.25 (dd, 1H). MS (ESI) 247.1 (M++H).

후처리

  1. customwas degassed by argon bubbling for 15 min.
  2. customdegassing
  3. additionwas added
  4. extractionextracted with EtOAc (3×30 mL)
  5. washthe combined extracts washed with brine
  6. dry with materialThe organic phase was dried over Na2SO4
  7. concentrationconcentrated in vacuo
  8. customThe crude residue was chromatographed on silica gel eluting with EtOAc:hexane (2:3)
  9. customto afford a white solid which
  10. customwas recrystallized from EtOAc/Hexane

출처 및 근거

ORD 기록
ord-02d28ef7874b4f34ade698dd79add9bd
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07569592B2

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