Sodium Hydroxide → 5-Methoxy-6-(trifluoromethyl)indoline
反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[C:12]([F:15])([F:14])[F:13])[NH:8][CH:7]=[CH:6]2.C([BH3-])#N.[Na+].[OH-].[Na+]>C(O)(=O)C.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[C:12]([F:15])([F:13])[F:14])[NH:8][CH2:7][CH2:6]2参加物
6
実験手順
The indole (D2) (67.63 g, 0.315 mol) in glacial acetic acid (500 ml) was treated with sodium cyanoborohydride (40 g, 0.637 mol) portionwise at room temperature with stirring. After 3 h at room temperature the reaction mixture was diluted with water (500 ml) and basified with 40% aqueous NaOH with cooling. The mixture was then extracted with dichloromethane (3×500 ml) and the combined extracts were dried (Na2SO4) and evaporated to give the title compound (67.73 g, 99%) as an off-white solid.
後処理
- temperaturewith cooling
- extractionThe mixture was then extracted with dichloromethane (3×500 ml)
- dry with materialthe combined extracts were dried (Na2SO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-073aa94d19c44708b81e9e62e6c7d586
- 出典データセット
- uspto-grants-2002_04
- 特許番号
- US06369060B1
反応ノート
読み込み中…