HRID27889
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
4.76 g 5,6-dihydro-6-methylaminomethyl-11H-dibenzo[b,e]azepine is dissolved in 125 ml dibromopropane and 5 ml triethylamine is added to the solution. The mixture is boiled under reflux with stirring for 2 hours, after which it is cooled. 150 ml Water is then added and the whole is shaken for a little while, after which the aqueous layer is separated from the dibromopropane layer. The organic layer is subsequently dried over sodium sulphate and evaporated to dryness under vacuum. The residue is further purified chromatographically on a silica gel column with methanol:acetone (9:1) as eluent.
WORKUP
后处理
- temperatureunder reflux
- temperatureafter which it is cooled
- stirringthe whole is shaken for a little while
- customafter which the aqueous layer is separated from the dibromopropane layer
- dry with materialThe organic layer is subsequently dried over sodium sulphate
- customevaporated to dryness under vacuum
- customThe residue is further purified chromatographically on a silica gel column with methanol:acetone (9:1) as eluent