反应详情

2 acetyl-9 benzyl-1,2,3,4-tetrahydro-β-carboline was prepared as follows: Under a nitrogen atmosphere, 8.0 mmol of 2 acetyl-1,2,3,4-tetrahydro-β-carboline (1.71 was dissolved in 4Q mL dry dimethylformamide (DMF). The solution was stirred over ice, and NaH (2 g) was added under N2. The suspension was stirred for 1 hour, and then benzylbromide (9.2 mmol, 1.56 was slowly to the cooled suspension. After a further 2 hours of stirring at ambient temperature, the mixture was filtered and the filtrate added to 320 mL 0.1 N HCl. Crude 2-acetyl- 9-benzyl-1,2,3,4-tetrahydro-β-carboline separated as an oil. The oil was collected by centrifugation, washed with water, and dried over anhydrous MgSO:. The product was purified by standard chromatographic procedures using a 60:40 mixture of ether:hexane.

1. additionwas added under N2
2. stirringAfter a further 2 hours of stirring at ambient temperature
3. filtrationthe mixture was filtered
4. additionthe filtrate added to 320 mL 0.1 N HCl
5. customCrude 2-acetyl- 9-benzyl-1,2,3,4-tetrahydro-β-carboline separated as an oil
6. customThe oil was collected by centrifugation
7. washwashed with water
8. dry with materialdried over anhydrous MgSO
9. customThe product was purified by standard chromatographic procedures
10. additiona 60:40 mixture of ether