HRID918249
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 2.5 g of 2-[ N-(2-norbornylmethyl)trichloroacetamido]-5-nitrobenzophenone in 50 ml of tert-butyl alcohol was added 2 g of ammonium acetate and the resulting mixture was heated under reflux for 7 hours. Then 2 g of ammonium acetate was added thereto and the reaction was continued for additional 8 hours. The solvent was removed under reduced pressure, and the residue was extracted with chloroform. The chloroform extract was washed with water, dried over anhydrous sodium sulfate, and evaporated to dryness. The residual oil was crystallized from a mixture of carbon tetrachloride and diethyl ether to give 1-(2-norbornylmethyl)-4-phenyl-6-nitro-2(1H)-quinazolinone, m.p. 160°C.
WORKUP
后处理
- temperaturethe resulting mixture was heated
- temperatureunder reflux for 7 hours
- customThe solvent was removed under reduced pressure
- extractionthe residue was extracted with chloroform
- extractionThe chloroform extract
- washwas washed with water
- dry with materialdried over anhydrous sodium sulfate
- customevaporated to dryness
- customThe residual oil was crystallized from a mixture of carbon tetrachloride and diethyl ether