HRID962511
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
A mixture of 2.05 g of 2-chloro-6,11-dihydro-5H-dibenz[b,e]azepine, 2.15 g of 4-nitrobenzoyl chloride, 1.50 g of N,N-diisopropylethylamine, 54 mg of 4-(dimethylamino)pyridine in 15 ml of dichloromethane is refluxed for 18 hours. The mixture is cooled and washed with H2O, 1N HCl, 1M NaHCO3, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the pad washed with dichloromethane. The filtrate is concentrated and the residue recrystallized from dichloromethane-hexane to give 2.33 g of crystals, m.p. 198°-201° C.
WORKUP
后处理
- temperatureis refluxed for 18 hours
- temperatureThe mixture is cooled
- washwashed with H2O, 1N HCl, 1M NaHCO3, brine
- dry with materialdried (Na2SO4)
- filtrationThe solution is filtered through a thin pad of hydrous magnesium silicate
- washthe pad washed with dichloromethane
- concentrationThe filtrate is concentrated
- customthe residue recrystallized from dichloromethane-hexane