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Pentafluoronitrobenzene → 1,2,4,5-Tetrafluoro-3-methoxy-6-nitrobenzene

HRID 352260
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HRID 352260 반응식
[F:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([F:11])[C:5]([F:12])=[C:4](F)[C:3]=1[F:14].[CH3:15][O-:16].[Na+]>CO>[F:1][C:2]1[C:3]([F:14])=[C:4]([O:16][CH3:15])[C:5]([F:12])=[C:6]([F:11])[C:7]=1[N+:8]([O-:10])=[O:9]
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참가 물질

4

반응물 2

HCID 70154PentafluoronitrobenzeneHCID 10942334Sodium Methoxide

생성물 1

HCID 42613721,2,4,5-Tetrafluoro-3-methoxy-6-nitrobenzene수율 72%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

50 g of pentafluoronitrobenzene was dissolved in 400 ml of dry methanol. Thereto was dropwise added, with ice-cooling, a solution of 13.95 g of sodium methoxide dissolved in 50 ml of dry methanol. A reaction was allowed to take place at room temperature for 2 hours. The reaction mixture was concentrated to a volume of about ⅓ under vacuum. The residue was poured into 500 ml of water. The organic layer was extracted with 300 ml of ether. The ether layer was washed with an aqueous sodium chloride solution and dried over MgSO4. The resulting solution was subjected to vacuum distillation to remove the solvent. The residue was subjected to vacuum distillation (96 to 97° C./0.35 mmHg (47 Pa)) to obtain 38 g of 2,3,5,6-tetrafluoro-4-methoxynitrobenzene (yield: 72%).

후처리

  1. additionThereto was dropwise added, with ice-
  2. temperaturecooling
  3. customat room temperature
  4. customfor 2 hours
  5. concentrationThe reaction mixture was concentrated to a volume of about ⅓ under vacuum
  6. additionThe residue was poured into 500 ml of water
  7. extractionThe organic layer was extracted with 300 ml of ether
  8. washThe ether layer was washed with an aqueous sodium chloride solution
  9. dry with materialdried over MgSO4
  10. distillationThe resulting solution was subjected to vacuum distillation
  11. customto remove the solvent
  12. distillationThe residue was subjected to vacuum distillation (96 to 97° C./0.35 mmHg (47 Pa))

출처 및 근거

ORD 기록
ord-9b4f7023777043d5a890227bde1e6aa3
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06746722B2

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