Potassium Carbonate → 4-Ethynyl-1-(2,2,2-trifluoroethyl)-1H-pyrazole
反応式
[F:1][C:2]([F:16])([F:15])[CH2:3][N:4]1[CH:8]=[C:7]([C:9]#[C:10][Si](C)(C)C)[CH:6]=[N:5]1.C(=O)([O-])[O-].[K+].[K+]>CO>[C:9]([C:7]1[CH:6]=[N:5][N:4]([CH2:3][C:2]([F:15])([F:16])[F:1])[CH:8]=1)#[CH:10]参加物
4
実験手順
1-(2,2,2-Trifluoroethyl)-4-((trimethylsilyl)ethynyl)-1H-pyrazole (Preparation 147, 1.19 g) was dissolved in methanol (7 ml) and potassium carbonate (30 mg) was added. The reaction was stirred at room temperature for 3.5 hours. The methanol was evaporated and the residue taken up in dichloromethane (20 ml) and filtered through a plug of silica eluting with DCM to afford the title compound (326 mg, 53%). 1H-NMR (CDCl3, 500 MHz): δ 3.06 (s, 1H), 4.70 (q, J=8.20 Hz, 2H), 7.69 (s, 1H), 7.70 (s, 1H). 19F-NMR (CDCl3, 470.385 MHz): −71.69
後処理
- customThe methanol was evaporated
- filtrationfiltered through a plug of silica eluting with DCM
出典と根拠
- ORDレコード
- ord-fb6067dfeed74c31b6985cce5654ac31
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09371319B2
反応ノート
読み込み中…