HRID364073
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
Here, 3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-1-chloropropane (10 g, 0.0336 mol) is heated to 130° C. for 3 hours with 2-(3,4-dimethoxyphenylamino)-ethylamine (13 g, 0.066 mol). After cooling, the reaction mixture is distributed between sodium hydroxide solution and methylene chloride. The organic phase is separated, dried over sodium sulfate and concentrated. The residue is chromatographed on silica gel (eluant: methylene chloride/methanol/conc. ammonia: 90/10/0.25). The product thus obtained is converted into the dihydrochloride in the usual way.
WORKUP
后处理
- temperatureAfter cooling
- customThe organic phase is separated
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customThe residue is chromatographed on silica gel (eluant: methylene chloride/methanol/conc. ammonia: 90/10/0.25)
- customThe product thus obtained