Trifluoroacetic acid → HCID 178506065、化合物
反応式
[Br: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.[OH-].[Na+]>[Br: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
実験手順
A solution of 5-bromo-N,N-dimethyl-3-(trifluoromethyl)-1H-pyrazole-1-sulfonamide (i.e. the product of Example 11, Step A) (4.50 g, 14.0 mmol) and trifluoroacetic acid (2.0 mL, 26 mmol) was stirred at 25° C. for 4 h. The reaction mixture was diluted with water (20 mL), and sodium hydroxide was added to raise the pH to 12. The solution was extracted with chloroform, dried (MgSO4), and concentrated under reduced pressure to give 2.73 g of the title compound as a yellow light oil. This compound was of sufficient purity to use in subsequent reactions.
後処理
- additionwas added
- temperatureto raise the pH to 12
- extractionThe solution was extracted with chloroform
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-e4191aa366d34869a418cddbd51ede09
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08642634B2
反応ノート
読み込み中…