HRID1087116
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5.5 g 2-(3- chloropropylthio)benzamide, 5.3 g of 4-[3-(ethylamino) -2-hydroxypropoxy]- benzonitrile, 6.6 g potassium carbonate and 7.2 g sodiumiodide were mixed in 100 ml of acetonitrile and heated to reflux for two days. The mixture was filtered and evaporated and the residue was dissolved in 1 M sulphuric acid. The acidic water layer was then washed twice with ether, alkalized with 10 M sodiumhydroxide and extracted with dichlormethane. The organic layer was dried over sodiumsulphate, treated with active carbon, filtered and evaporated. The residue, 8.7 g, was separated by column chromatography. Yield: 4.5 g of the title compound.
WORKUP
后处理
- temperatureheated
- temperatureto reflux for two days
- filtrationThe mixture was filtered
- customevaporated
- dissolutionthe residue was dissolved in 1 M sulphuric acid
- washThe acidic water layer was then washed twice with ether
- extractionextracted with dichlormethane
- dry with materialThe organic layer was dried over sodiumsulphate
- additiontreated with active carbon
- filtrationfiltered
- customevaporated
- customThe residue, 8.7 g, was separated by column chromatography