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
Into a 250 ml flask, provided with a reflux condenser, were introduced 10 g of 2,3,5-trichlorobenzoyl chloride in 20 ml of anhydrous C6H6, a solution of 5.3 g of di-sec.butylamine in 7 ml of anhydrous C6H6 and 5 g of triethylamine. This mass was then heated to reflux temperature for about 1 hour. Thereupon it was left to cool down to room temperature and the solvent was removed under reduced pressure in a rotating evaporator. The mass was then washed with acidulated H2O, with H2O and was then extracted with ethyl ether. The etheric extract was then dried on anhydrous Na2SO4, filtered and the solvent removed under reduced pressure. 12.6 g of yellowing crystals of 2,3,5-trichloro-N,N-di-sec.butyl-benzamide were obtained.
WORKUP
后处理
- customInto a 250 ml flask, provided with a reflux condenser
- temperatureThis mass was then heated
- temperatureto reflux temperature for about 1 hour
- waitThereupon it was left
- customthe solvent was removed under reduced pressure in a rotating evaporator
- washThe mass was then washed with acidulated H2O, with H2O
- extractionwas then extracted with ethyl ether
- extractionThe etheric extract
- dry with materialwas then dried on anhydrous Na2SO4
- filtrationfiltered
- customthe solvent removed under reduced pressure
- customwere obtained