1,1,1-Trifluoro-2-iodoethane → 4-Iodo-1-(2,2,2-trifluoroethyl)-1H-pyrazole
反応式
[I:1][C:2]1[CH:3]=[N:4][NH:5][CH:6]=1.[F:7][C:8]([F:12])([F:11])[CH2:9]I>CN(C=O)C>[I:1][C:2]1[CH:3]=[N:4][N:5]([CH2:9][C:8]([F:12])([F:11])[F:7])[CH:6]=1参加物
4
反応条件
- 温度
- 60 °C
実験手順
A mixture of 4-iodo-1H-pyrazole (960 mg, 5 mmol), 2,2,2-trifluoroethyl iodide (3.13 g, 15 mmol) and CS2CO3 (2.4 g, 7.7 mmol) in DMF (5 ml) is heated at 60° C. with stirring overnight. After cooling, the reaction mixture is partitioned between water (50 ml) and ether (20 ml). The organic layer is separated, dried (MgSO4) and concentrated to afford the title compound as an oil which solidified upon standing 1.0 g (72%). 1HNMR (CDCl3): δ (ppm) 4.70 (m, 2H), 7.56 (s, 1H), 7.59 (s, 1H).
後処理
- temperatureAfter cooling
- customthe reaction mixture is partitioned between water (50 ml) and ether (20 ml)
- customThe organic layer is separated
- dry with materialdried (MgSO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-12ed34ecab0740fe9a80eddc787edeb3
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07705030B2
反応ノート
読み込み中…