Nitric Acid → 4,5-Difluoro-2-nitrobenzaldehyde

HRID 55353노트

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HRID 55353 반응식
S(=O)(=O)(O)O.[F:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:14]=1[F:15])[CH:10]=[O:11].[N+:16]([O-])([OH:18])=[O:17]>>[F:6][C:7]1[CH:8]=[C:9]([C:12]([N+:16]([O-:18])=[O:17])=[CH:13][C:14]=1[F:15])[CH:10]=[O:11]

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 5880883,4-Difluorobenzaldehyde

생성물 1

HCID 199572974,5-Difluoro-2-nitrobenzaldehyde

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온도
5 °C

실험 절차

To 520 cm3 of sulphuric acid, cooled to 0° C., are added, with stirring, 60 cm3 of fuming nitric acid, over 30 minutes. 100 g of 3,4-difluorobenzaldehyde are added over 30 minutes at approximately 0° C. to the solution obtained. The temperature is allowed to return to approximately 20° C. and stirring is continued for 3 hours at this temperature. After cooling to approximately 5° C., the reaction mixture is poured, over 30 minutes and with vigorous stirring, onto 1200 g of crushed ice. The temperature is allowed to return to approximately 20° C., followed by extraction with twice 600 cm3 of toluene. The combined organic extracts are washed with 3 times 1000 cm3 of water, and concentrated under reduced pressure (20 kPa) at 50° C. 113 g of 3,4-difluoro-6-nitrobenzaldehyde are obtained in the form of a brown oil, which is used as it is in the subsequent syntheses. A purified sample of 3,4-difluoro-6-nitrobenzaldehyde gives the following characteristics:

후처리

  1. additionare added
  2. customobtained
  3. customto return to approximately 20° C.
  4. stirringstirring
  5. customto return to approximately 20° C.
  6. extractionfollowed by extraction with twice 600 cm3 of toluene
  7. washThe combined organic extracts are washed with 3 times 1000 cm3 of water
  8. concentrationconcentrated under reduced pressure (20 kPa) at 50° C

출처 및 근거

ORD 기록
ord-eddde3e0a98249119dc51c1baddd3cbe
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624933

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