Nitric Acid → HCID 178526837, 화합물

HRID 573188

반응식

HRID 573188 반응식
[F:1][C:2]([F:11])([F:10])[C:3]1[C:4]([OH:9])=[N:5][CH:6]=[CH:7][CH:8]=1.S(=O)(=O)(O)O.[N+:17]([O-])([OH:19])=[O:18]>>[N+:17]([C:7]1[CH:8]=[C:3]([C:2]([F:1])([F:10])[F:11])[C:4]([OH:9])=[N:5][CH:6]=1)([O-:19])=[O:18]

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 36784112(1H)-Pyridinone, 3-(trifluoromethyl)-

생성물 1

HCID 178526837HCID 178526837, 화합물

반응 조건

온도
0 °C

실험 절차

3-(Trifluoromethyl)pyridin-2-ol (2.3 g) was added to concentrated sulfuric acid (15 mL) at 0° C. The mixture was stirred at 0° C. for 5 minutes. To this solution was added nitric acid (fuming, 6 mL) dropwise over 5 minutes. The reaction mixture was stirred at room temperature for 2 hours, and then heated at 50° C. for 3 hours. After cooling, the reaction mixture was poured into ice (200 g), and the mixture was extracted with ethyl acetate three times. The combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure to give the title compound.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 2 hours
  2. temperatureheated at 50° C. for 3 hours
  3. temperatureAfter cooling
  4. extractionthe mixture was extracted with ethyl acetate three times
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-86570945c10448b6b884dda0ab05615e
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029404B2

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