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Nitric Acid → 3-Nitro-5-pentafluorosulfanylbenzoic Acid

HRID 217757
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HRID 217757 반응식
[F:1][S:2]([F:15])([F:14])([F:13])([F:12])[C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7].S(=O)(=O)(O)O.[N+:21]([O-])([OH:23])=[O:22]>>[F:1][S:2]([F:12])([F:13])([F:14])([F:15])[C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:21]([O-:23])=[O:22])[CH:11]=1)[C:6]([OH:8])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric Acid2회HCID 27792093-(Pentafluorosulfanyl)benzoic acid

생성물 1

HCID 596421523-Nitro-5-pentafluorosulfanylbenzoic Acid

실험 절차

3-Pentafluorosulfanylbenzoic acid (15 g) was dissolved in fuming nitric acid (120 ml) and stirred at RT with exclusion of moisture. Then concentrated sulfuric acid (7.5 ml) was added and the mixture was stirred at 75° C. After stirring at 75° C. for 8 h, the mixture was left to stand overnight, then further sulfuric acid (1.5 ml) was added and the mixture was heated to 75° C. while stirring for 8 h. After being left to stand overnight, the mixture was added to ice-water and stirred for 2 h. Then the precipitate was filtered off with suction and dried under high vacuum. 13.7 g of 3-pentafluorosulfanyl-5-nitrobenzoic acid were obtained.

후처리

  1. stirringthe mixture was stirred at 75° C
  2. stirringAfter stirring at 75° C. for 8 h
  3. waitthe mixture was left
  4. temperaturethe mixture was heated to 75° C.
  5. stirringwhile stirring for 8 h
  6. waitAfter being left
  7. waitto stand overnight
  8. stirringstirred for 2 h
  9. filtrationThen the precipitate was filtered off with suction
  10. customdried under high vacuum

출처 및 근거

ORD 기록
ord-a6c5d621f47346a6b52aeafa8c89132e
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08198272B2

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