Water → 3-(3-(Dimethylamino)propyl)-4,5,6,7-tetrahydro-1H-indole-2-carbaldehyde
反応式
P(Cl)(Cl)(Cl)=O.[CH3:6][N:7]([CH3:20])[CH2:8][CH2:9][CH2:10][C:11]1[C:19]2[CH2:18][CH2:17][CH2:16][CH2:15][C:14]=2[NH:13][CH:12]=1.O.[OH-].[Na+].CN(C)[CH:26]=[O:27]>>[CH3:20][N:7]([CH3:6])[CH2:8][CH2:9][CH2:10][C:11]1[C:19]2[CH2:18][CH2:17][CH2:16][CH2:15][C:14]=2[NH:13][C:12]=1[CH:26]=[O:27]参加物
実験手順
Phosphorus oxychloride (9.2 g, 0.06 mol) was slowly added to 12 ml of dimethylformamid at 0° C. with stirring and the mixture stirred for 30 minutes. Dimethyl-[3-(4,5,6,7-tetrahydro-1H-indol-3-yl)-propyl]-amine ( 6.2 g, 0.03 mol) was dissolved in 10 ml of dimethylformamide and added to the mixture. The reaction was stirred for 2 hours at room temperature. The stirred mixture was cooled in an ice bath and water was slowly added followed by 10 N sodium hydroxide solution until pH was 10. The mixture was stirred at room temperature for 45 minutes and extracted with ethyl acetate. The ethyl acetate extract was washed with brine, dried over anhydrous sodium sulfate and concentrated to give 3-(3-dimethylamino-propyl)-4,5,6,7-tetrahydro-1H-indole-2-carbaldehyde (3.5 g, 50% yield).
後処理
- stirringthe mixture stirred for 30 minutes
- additionadded to the mixture
- stirringThe reaction was stirred for 2 hours at room temperature
- temperatureThe stirred mixture was cooled in an ice bath
- stirringThe mixture was stirred at room temperature for 45 minutes
- extractionextracted with ethyl acetate
- extractionThe ethyl acetate extract
- washwas washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-697eb5930a154623affff4edb8b60fb5
- 出典データセット
- uspto-grants-2004_08
- 特許番号
- US06777417B2
反応ノート
読み込み中…