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

HRID 1528538ノート

反応式

HRID 1528538 の反応式
[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

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 674628085-chloro-N,N-dimethyl-3-(trifluoromethyl)-1H-pyrazole-1-sulfonamide2 回

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 10340Sodium Carbonate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a7d470f882d34cc6b45d0ea4fa868cdc
出典データセット
uspto-grants-2015_07
特許番号
US09090604B2

反応ノート

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