Guaiacol → N-[2-fluoro-5-(2-methoxyphenoxy)-4-nitrophenyl]acetamide

HRID 493935노트

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HRID 493935 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[OH:9].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.[F:21][C:22]1[CH:27]=[C:26]([N+:28]([O-:30])=[O:29])[C:25](F)=[CH:24][C:23]=1[NH:32][C:33](=[O:35])[CH3:34]>O>[F:21][C:22]1[CH:27]=[C:26]([N+:28]([O-:30])=[O:29])[C:25]([O:9][C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[O:2][CH3:1])=[CH:24][C:23]=1[NH:32][C:33](=[O:35])[CH3:34]

참가 물질

6

반응물 4

HCID 460GuaiacolHCID 6228Dimethylformamide2회HCID 11430Potassium CarbonateHCID 14624893N-(2,5-Difluoro-4-nitrophenyl)acetamide

생성물 1

HCID 21933575N-[2-fluoro-5-(2-methoxyphenoxy)-4-nitrophenyl]acetamide수율 86.6%

시약·촉매·용매 1

HCID 962Water용매

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온도
60 °C

실험 절차

First, 2.73 g of 2-methoxyphenol and 5.5 g of potassium carbonate were added to 20 ml of N,N-dimethylformamide, and the temperature was increased to 60° C. To the mixture was added dropwise a solution consisting of 4.3 g of N-(2,5-difluoro-4-nitrophenyl)acetamide and 30 ml of N,N-dimethylformamide at a temperature of 60° C. to 65° C. After stirring while keeping the temperature for 1 hour, the mixture was cooled to room temperature and then poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with diluted hydrochloric acid and water, dried over magnesium sulfate, and then concentrated to give 5.52 g of N-[2-fluoro-5-(2-methoxyphenoxy)-4-nitrophenyl]acetamide.

후처리

  1. additionTo the mixture was added dropwise a solution
  2. customfor 1 hour
  3. temperaturethe mixture was cooled to room temperature
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with diluted hydrochloric acid and water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9d069d5261694b7f90b957e86a5df2cd
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538072B2

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