Nitric Acid → 1-(2,6-Difluoro-3-nitrophenyl)ethanone

HRID 571697

반응식

HRID 571697 반응식
OS(O)(=O)=O.[N+:6]([O-:9])(O)=[O:7].[F:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:12]=1[C:18](=[O:20])[CH3:19]>C(Cl)Cl>[F:10][C:11]1[C:16]([N+:6]([O-:9])=[O:7])=[CH:15][CH:14]=[C:13]([F:17])[C:12]=1[C:18](=[O:20])[CH3:19]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 836431-(2,6-Difluorophenyl)ethan-1-one

생성물 1

HCID 138536371-(2,6-Difluoro-3-nitrophenyl)ethanone

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-40 °C

실험 절차

To a −40° C. mixture of concentrated H2SO4 (100 mL) and fuming HNO3 (100 mL) was added 1-(2,6-difluorophenyl)ethanone (20 g, 128 mmol) dropwise. The resulting mixture was stirred at −40° C. for 2 h then poured slowly onto ice. That mixture was diluted with DCM and the phases were separated. The aqueous layer was neutralized with sat. aq. NaHCO3 and then extracted with DCM. All organic portions were combined, dried over MgSO4, filtered, and concentrated to give 1-(2,6-difluoro-3-nitrophenyl)ethanone (26.3 g, 131 mmol, >theoretical) that was used without further purification.

후처리

  1. additionthen poured slowly onto ice
  2. customthe phases were separated
  3. extractionextracted with DCM
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fdffe23e2db44304b83f1530697be30a
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029362B2

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