HRID364070
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
First 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one (131.5 g, 0.6 mol) is suspended in dimethylsulfoxide (900 ml) and mixed with potassium tert.butoxide (80.8 g, 0.72 mol) with stirring. After 10 minutes the solution obtained is added dropwise to 1-bromo-3-chloropropane (77 ml, 0.72 mol) in dimethylsulfoxide (300 ml), while cooling with ice water. After an hour the mixture is poured onto ice water. After a short time the greasy precipitate begins to crystallize. The precipitate is suction filtered, dissolved in acetone, precipitated again water water, suction filtered and dried.
WORKUP
后处理
- customAfter 10 minutes the solution obtained
- additionAfter an hour the mixture is poured onto ice water
- customto crystallize
- filtrationfiltered
- dissolutiondissolved in acetone
- customprecipitated again water water, suction
- filtrationfiltered
- customdried