4-Methylmorpholine → 1H-Inden-2-amine, 5-bromo-2,3-dihydro-, (2R)-
反応式
Br.[Br:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[CH2:8][CH:7]([NH2:12])[CH2:6]2.CN1CCOCC1>CO>[Br:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[CH2:8][C@@H:7]([NH2:12])[CH2:6]2参加物
4
反応条件
- 温度
- 60 °C
実験手順
25 g of 5-bromo-indan-2-ylamine hydrobromide (85.32 mmol) and 9.85 ml of 4-methylmorpholin (89.59 mmol) were dissolved in 53 ml of methanol. The mixture was heated to 60° C. and a solution of 25.77 g of (1S)-(+)-campher-10-sulfonic acid (110.92 mmol) in 42 ml of methanol added within 25 minutes. The reaction mixture was stirred for 10 minutes at 60° C. and then allowed to cool down to room temperature over a 2 h time period, with stirring continuing for another 2 h. The precipitate was filtered, washed twice with 20 ml of ethyl acetate/methanol (2:1) and 20 ml of water, and finally dried at 50° C. under vacuo for 15 h to give 13.3 g of the salt.