反応式
FC(F)(F)C(O)=O.[F:8][C:9]1[C:14]([F:15])=[CH:13][CH:12]=[CH:11][C:10]=1[C@H:16]1[CH2:22][N:21]([CH2:23][CH2:24][S:25][CH3:26])[C:20](=[O:27])[C@H:19]([NH:28]C(=O)OC(C)(C)C)[CH2:18][CH2:17]1>ClCCl>[NH2:28][C@@H:19]1[CH2:18][CH2:17][C@@H:16]([C:10]2[CH:11]=[CH:12][CH:13]=[C:14]([F:15])[C:9]=2[F:8])[CH2:22][N:21]([CH2:23][CH2:24][S:25][CH3:26])[C:20]1=[O:27]参加物
4
実験手順
Trifluoroacetic acid (2 mL) was added to a solution of tert-butyl (3R,6S)-6-(2,3-difluorophenyl)-1-[2-(methylthio)ethyl]-2-oxoazepan-3-ylcarbamate (77 mg, 0.186 mmol) in dichloromethane (10 mL). After 30 min, the solution was concentrated and azeotroped with toluene (2×). Saturated aqueous sodium bicarbonate solution was added and the mixture was extracted with dichloromethane (3×). The combined organic extracts were washed with saturated brine, dried over magnesium sulfate, filtered and concentrated. MS 315.2 (M+1).
後処理
- concentrationthe solution was concentrated
- customazeotroped with toluene (2×)
- additionSaturated aqueous sodium bicarbonate solution was added
- extractionthe mixture was extracted with dichloromethane (3×)
- washThe combined organic extracts were washed with saturated brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-a96ed3d3e6f94316898a069fbedfb99e
- 出典データセット
- uspto-grants-2005_10
- 特許番号
- US06953790B2
関連ノート
読み込み中…