HRID365284
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
To a solution of N-(4-bromobenzyl)-N-(pyridin-2-yl)pro-pane-1,3-diamine (1.0 g, 3.123 mmol) in chloroform (40 ml) was added 3-morpholinopropyl isothiocyanate (593 mg, 3.123 mmol) and the reaction mixture was stirred for 20 h at reflux temperature. To the reaction mixture was added 10 drops of 3-morpholinopropyl isothiocyanate and the reaction mixture was stirred for an additional 4 h at reflux temperature. The volatiles were evaporated in vacuo and the residue (2.05 g) was dissolved in ethyl acetate (20 ml) and left over night at room temperature. The precipitate was filtered off and washed with ethyl acetate and dried affording 1.20 g (76%) of the title compound as a solid.
WORKUP
后处理
- temperatureat reflux temperature
- stirringthe reaction mixture was stirred for an additional 4 h
- temperatureat reflux temperature
- customThe volatiles were evaporated in vacuo
- dissolutionthe residue (2.05 g) was dissolved in ethyl acetate (20 ml)
- waitleft over night at room temperature
- filtrationThe precipitate was filtered off
- washwashed with ethyl acetate
- customdried