2,5-Dichlorophenol → 1-(2,5-Dichloro-phenoxy)-2-fluoro-4-nitro-benzene

HRID 33758

反応式

HRID 33758 の反応式
[F:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1F.[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=1[OH:20].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=1[O:20][C:7]1[CH:6]=[CH:5][C:4]([N+:9]([O-:11])=[O:10])=[CH:3][C:2]=1[F:1]

参加物

5

反応物 3

HCID 662,5-DichlorophenolHCID 11430Potassium CarbonateHCID 1230531,2-Difluoro-4-nitrobenzene

生成物 1

HCID 597980461-(2,5-Dichloro-phenoxy)-2-fluoro-4-nitro-benzene収率 94.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

A mixture of 3,4-difluoronitrobenzene (3.2 g, 0.02 mol), 2,5-dichlorophenol (3.59 g, 0.022 mol), and potassium carbonate (3.0 g, 0.022 mol) in 25 ml of anhydrous DMF was heated to 150° C. with stirring overnight. After cooling to room temperature, the reaction mixture was poured into 500 ml of ice water and stirred for 30 min. The precipitates were collected by filtration, washed with water, and dried in vacuo to give 5.72 g (94.7%) of crude product.

後処理

  1. temperatureAfter cooling to room temperature
  2. stirringstirred for 30 min
  3. filtrationThe precipitates were collected by filtration
  4. washwashed with water
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-fafef133eb40479aaefe077d5315a767
出典データセット
uspto-grants-2008_09
特許番号
US07429667B2

関連ノート

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