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

HRID 33758

반응식

HRID 33758 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fafef133eb40479aaefe077d5315a767
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429667B2

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