Potassium Carbonate → 2-(4-Bromo-2-chloro-6-methylphenoxy)-5-nitropyridine

HRID 1023341ノート

反応式

HRID 1023341 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[OH:10].Cl[C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][N:13]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Br:8][C:6]1[CH:5]=[C:4]([CH3:9])[C:3]([O:10][C:12]2[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][N:13]=2)=[C:2]([Cl:1])[CH:7]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 783082-Chloro-5-nitropyridineHCID 820314-Bromo-6-chloro-o-cresol

生成物 1

HCID 673279772-(4-Bromo-2-chloro-6-methylphenoxy)-5-nitropyridine収率 99.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

To a DMF (30 mL) solution of 2-chloro-4-bromo-6-methylphenol (4.90 g) were added 2-chloro-5-nitropyridine (3.58 g) and K2CO3 (3.12 g) at room temperature. After stirring at 50° C. for 3 hours, the solvent was removed under reduced pressure. To the residue was added water, and extracted with AcOEt. The organic layer was washed with water, saturated aqueous NaCl, dried over anhydrous Na2SO4, and concentrated under reduced pressure to give 2-(4-bromo-2-chloro-6-methylphenoxy)-5-nitropyridine as a brown solid (7.59 g).

後処理

  1. customthe solvent was removed under reduced pressure
  2. additionTo the residue was added water
  3. extractionextracted with AcOEt
  4. washThe organic layer was washed with water, saturated aqueous NaCl
  5. dry with materialdried over anhydrous Na2SO4
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-ab31265ad4554752ba00e1fb55154b71
出典データセット
uspto-grants-2014_05
特許番号
US08722663B2

反応ノート

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