p-Fluoronitrobenzene → HCID 22569398、化合物

HRID 1110332ノート

反応式

HRID 1110332 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[CH3:11][N:12]([CH3:16])[CH2:13][CH2:14][NH2:15].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[CH3:11][N:12]([CH3:16])[CH2:13][CH2:14][NH:15][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 9590p-FluoronitrobenzeneHCID 11430Potassium CarbonateHCID 66053N,N-Dimethylethylenediamine

生成物 1

HCID 22569398HCID 22569398、化合物収率 90%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a stirred solution of 4-fluoronitrobenzene (7 g, 50 mmol), N,N-dimethylethylenediamine (5.2 g, 60 mmol) and potassium carbonate (7 g, 50 mmol) in 25 ml of dimethysulfoxide was added 0.2 g of tris(3,6-dioxaheptyl) amine(TDA-1). The heterogenous mixture was heated at 90° for 2 h. After cooling to room temperature, 100 g of crushed ice was added to precipitate out the yellow product in 90% yield (9.4 g, 45 mmol).

後処理

  1. temperatureThe heterogenous mixture was heated at 90° for 2 h
  2. customto precipitate out the yellow product in 90% yield (9.4 g, 45 mmol)

出典と根拠

ORDレコード
ord-cc816448f022489481868fbb30556924
出典データセット
uspto-grants-1990_12
特許番号
US04975092

反応ノート

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