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Potassium Carbonate → 4-(4-Chlorophenyl)-3-nitropyridine

HRID 2214339
ノート
印刷プレビュー

反応式

HRID 2214339 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[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+]>C(COC)OC.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>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([C:2]2[CH:7]=[CH:6][N:5]=[CH:4][C:3]=2[N+:8]([O-:10])=[O:9])=[CH:14][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 742994-Chlorophenylboronic acidHCID 27357814-Chloro-3-nitropyridine

生成物 1

HCID 219471174-(4-Chlorophenyl)-3-nitropyridine

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 8071
1,2-Dimethoxyethane
溶媒

実験手順

In a sulfonation flask 6.9 g (44 mmol) of 4-chloro-3-nitropyridine, 6.5 g (42 mmol) 4-chloro-phenylboronic acid, 6.0 g (44 mmol) potassium carbonate (saturated solution in water) and 1.0 g (0.9 mmol) tetrakis(triphenylphosphine)palladium are dissolved in 100 ml of dimethoxyethane (DME). The mixture is heated under reflux conditions under a constant nitrogen stream for 5 hours. Then the solvent is removed in a water jet vacuum and the residue taken up in ethylacetate. The organic phase is washed twice with water and after drying of the organic phase with sodium sulfate, the solvent is removed in a water jet vacuum. The resulting crude product is purified by column chromatography over silica gel (eluant: hexane/ethylacetate 1:1). Yield: 8.9 g 4-(4′-chlorophenyl)-3-nitropyridine in the form of brownish crystals; m.p. 74–76° C.

後処理

  1. temperatureThe mixture is heated under reflux conditions under a constant nitrogen
  2. customThen the solvent is removed in a water jet vacuum
  3. washThe organic phase is washed twice with water
  4. dry with materialafter drying of the organic phase with sodium sulfate
  5. customthe solvent is removed in a water jet vacuum
  6. customThe resulting crude product is purified by column chromatography over silica gel (eluant: hexane/ethylacetate 1:1)

出典と根拠

ORDレコード
ord-a17dce72e04f4cf88382b071102640a5
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07109150B2

反応ノート

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