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Potassium Carbonate → HCID 9921211, 화합물

HRID 2213324
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HRID 2213324 반응식
[NH:1]1[CH:5]=[N:4][C:3]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=2)=[N:2]1.C(=O)([O-])[O-].[K+].[K+].F[C:19]1[CH:20]=[C:21]([CH:24]=[CH:25][CH:26]=1)[C:22]#[N:23]>CN(C=O)C>[N:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[C:3]1[N:4]=[CH:5][N:1]([C:19]2[CH:20]=[C:21]([CH:24]=[CH:25][CH:26]=2)[C:22]#[N:23])[N:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 678803-FluorobenzonitrileHCID 178420161HCID 178420161, 화합물

생성물 1

HCID 9921211HCID 9921211, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
145 °C

실험 절차

2-(1H-1,2,4-Triazol-3-yl)pyridine (0.24 g, 1.6 mmol), potassium carbonate (0.45 g, 3.2 mmol) and 3-fluorobenzonitrile (0.20 g, 1.6 mmol) were stirred in DMF (20 mL) at ambient temperature. The resulting reaction mixture was heated at 145° C. for 16 h, after which time it was quenched with H2O (30 mL) and diluted with EtOAc (200 mL). The EtOAc solution was washed with H2O (3×100 mL), then brine (100 mL) and dried (MgSO4), filtered, and concentrated in vacuo. The resulting residue was chromatographed on silica gel eluting with hexane:EtOAc (40:60) to afford 3-(3-pyridin-2-yl-1H-1,2,4-triazol-1-yl)benzonitrile as a white solid.

후처리

  1. customThe resulting reaction mixture
  2. customafter which time it was quenched with H2O (30 mL)
  3. additiondiluted with EtOAc (200 mL)
  4. washThe EtOAc solution was washed with H2O (3×100 mL)
  5. dry with materialbrine (100 mL) and dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe resulting residue was chromatographed on silica gel eluting with hexane:EtOAc (40:60)

출처 및 근거

ORD 기록
ord-9ad3c0d5134a412b8df25da103bfbd1c
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07105548B2

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