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

HRID 1023341노트

반응식

HRID 1023341 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ab31265ad4554752ba00e1fb55154b71
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722663B2

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