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Potassium Carbonate → HCID 9921211、化合物

HRID 2213324
ノート
印刷プレビュー

反応式

HRID 2213324 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 678803-FluorobenzonitrileHCID 178420161HCID 178420161、化合物

生成物 1

HCID 9921211HCID 9921211、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
145 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-9ad3c0d5134a412b8df25da103bfbd1c
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07105548B2

反応ノート

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