HRID1109159
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 1.00 g (0.005 mol) of rac-cis-2,3,3a,4,5,9b-Hexahydro-6-methoxy-1H-benzo[e]indole in 60 ml of ethyl methyl ketone was treated with 0.86 g (0.006 mol) of potassium carbonate, 0.29 g (0.002 mol) of sodium iodide and 1.50 g (0.005 mol) of N-(5-bromopentyl)phthalimide. The mixture was heated under reflux for 24 hours and, after cooling, treated with water. The mixture was extracted with ethyl acetate, the extracts were dried with sodium sulphate and the solvent was distilled off in a vacuum. Chromatography over silica gel with methylene chloride/methanol 20:1 gave 1.97 g (95%) of rac-N-[5-(cis-1,2,3a, 4,5,9b-hexahydro-6-methoxy-3H-benzo[e]indol-3-yl)pentyl]phthalimide.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 24 hours
- temperatureafter cooling
- extractionThe mixture was extracted with ethyl acetate
- dry with materialthe extracts were dried with sodium sulphate
- distillationthe solvent was distilled off in a vacuum