Water → 4-(4-Bromophenoxy)-2,5-dimethylnitrobenzene

HRID 405003ノート

反応式

HRID 405003 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl[C:16]1[C:21]([CH3:22])=[CH:20][C:19]([N+:23]([O-:25])=[O:24])=[C:18]([CH3:26])[CH:17]=1.O>CN(C)C=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:16]2[C:21]([CH3:22])=[CH:20][C:19]([N+:23]([O-:25])=[O:24])=[C:18]([CH3:26])[CH:17]=2)=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 78084-BromophenolHCID 11430Potassium CarbonateHCID 2527931-Chloro-2,5-dimethyl-4-nitrobenzene

生成物 1

HCID 685953564-(4-Bromophenoxy)-2,5-dimethylnitrobenzene収率 68.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

37.5 g (216.7 mmol) of 4-bromophenol and 35.4 g (256.2 mmol) of potassium carbonate are suspended in 500 ml of N,N-dimethylformamide and the suspension is stirred at room temperature for 1 h, before 36.6 g (197.0 mmol) of 4-chloro-2,5-dimethylnitrobenzene are added. The mixture is subsequently stirred at 150° C. for 14 h, water is added, and repeated extraction is carried out with ethyl acetate. The extracts are dried over Na2SO4 and filtered and the solvent is removed under reduced pressure. This is followed by purification by column chromatography (48.0 g, purity 91.0%, yield 68.8%, log P (pH 2.3)=4.86).

後処理

  1. additionare added
  2. extractionextraction
  3. dry with materialThe extracts are dried over Na2SO4
  4. filtrationfiltered
  5. customthe solvent is removed under reduced pressure
  6. customThis is followed by purification by column chromatography (48.0 g, purity 91.0%, yield 68.8%, log P (pH 2.3)=4.86)

出典と根拠

ORDレコード
ord-57c2386e089940c09c2e46307af27afd
出典データセット
uspto-grants-2014_06
特許番号
US08748662B2

反応ノート

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