Hydrofluoric Acid → HCID 13560838、化合物
反応式
[CH3:1][NH:2][S:3]([CH2:6][C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[NH:12][C:11]([Si](C)(C)C)=[CH:10]2)(=[O:5])=[O:4].F>CC#N>[CH3:1][NH:2][S:3]([CH2:6][C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[NH:12][CH:11]=[CH:10]2)(=[O:5])=[O:4]参加物
4
実験手順
5-[[(Methylamino)sulfonyl]methyl]-2-(trimethylsilyl)-1H-indole (4) (1.0 g, 0.00356 mol) was dissolved in CH3CN (40 mL). Concentrated hydrofluoric acid (HF, 1 mL) was added and the mixture was stirred at RT for 3 h. The solvent was removed in vacuo and the residue was dissolved in EtOAc. The organic phase was extracted sequentially with saturated aqueous NaHCO3 and brine, dried over MgSO4, filtered and concentrated in vacuo. Silica gel chromatography (10-100% EtOAc gradient in hexane) of the residue gave the product (5) (0.52 g, 65.2%).
後処理
- customThe solvent was removed in vacuo
- dissolutionthe residue was dissolved in EtOAc
- extractionThe organic phase was extracted sequentially with saturated aqueous NaHCO3 and brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-a5519c5e87a447118ed15e1b31d8a610
- 出典データセット
- uspto-grants-1996_12
- 特許番号
- US05583149
反応ノート
読み込み中…