4-But-2-ynyloxy-benzenesulfonyl chloride → 4-But-2-ynyloxybenzenesulfonyl fluoride
反応式
[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][C:9]([S:12](Cl)(=[O:14])=[O:13])=[CH:8][CH:7]=1)[C:2]#[C:3][CH3:4].[F-:16].[K+].[F-].[F-].[Ca+2]>>[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][C:9]([S:12]([F:16])(=[O:14])=[O:13])=[CH:8][CH:7]=1)[C:2]#[C:3][CH3:4]参加物
3
実験手順
To a solution of 4-but-2-ynyloxybenzenesulfonyl chloride (prepared from Example 30, step 4) (2.0 g, 8.18 mmol) in acetonitrle (10 ml) was added KF-CaF2 (2.85 g, 16.3 mmol) and the resulting mixture was stirred for 4 hours at room temperature. The reaction mixture was filtered and the filterate was concentrated. The crude product was dissolved in EtOAc and washed with water. The organic layer was dried over anhydrous Na2SO4 and the solvent was removed to obtain 1.5 g (80%) of the product as solid.
後処理
- filtrationThe reaction mixture was filtered
- concentrationthe filterate was concentrated
- dissolutionThe crude product was dissolved in EtOAc
- washwashed with water
- dry with materialThe organic layer was dried over anhydrous Na2SO4
- customthe solvent was removed
出典と根拠
- ORDレコード
- ord-62efb4c525574cd2adbb7c5d4b559db0
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06358980B1
反応ノート
読み込み中…