Trifluoroacetic acid → 5-chloro-3-(trifluoromethyl)-1H-pyrazole

HRID 238673노트

반응식

HRID 238673 반응식
[Cl:1][C:2]1[N:6](S(N(C)C)(=O)=O)[N:5]=[C:4]([C:13]([F:16])([F:15])[F:14])[CH:3]=1.FC(F)(F)C(O)=O>O.C(=O)([O-])[O-].[Na+].[Na+]>[Cl:1][C:2]1[NH:6][N:5]=[C:4]([C:13]([F:16])([F:15])[F:14])[CH:3]=1

참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acidHCID 674628085-chloro-N,N-dimethyl-3-(trifluoromethyl)-1H-pyrazole-1-sulfonamide2회

생성물 1

HCID 1785061975-chloro-3-(trifluoromethyl)-1H-pyrazole

시약·촉매·용매 2

HCID 962Water용매HCID 10340Sodium Carbonate용매

실험 절차

A solution of 5-chloro-N,N-dimethyl-3-(trifluoromethyl)-1H-pyrazole-1-sulfonamide (i.e. the product of Example 10, Step B) (4.38 g, 15.8 mmol) and trifluoroacetic acid (2.7 mL, 35 mmol) was stirred at 0° C. for 1.5 h. The reaction mixture was diluted with water (15 mL), and sodium carbonate was added to raise the pH to 12. The solution was extracted with diethyl ether, dried (MgSO4), and concentrated under reduced pressure to give 2.1 g of the title compound. This compound was of sufficient purity to use in subsequent reactions.

후처리

  1. additionwas added
  2. temperatureto raise the pH to 12
  3. extractionThe solution was extracted with diethyl ether
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-cede304086f944cc80ebed391f7dfdf4
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642634B2

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