HRID903424
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 slurry of 21.80 g. of 2-bromopropylamine hydrobromide in 200 ml. of glyme at 3° C. is added a solution of 23.96 g. of 4-(8-cyclohexyloctylamino)benzoyl chloride hydrochloride in 65 ml. of glyme, concurrently with 26 ml. of triethylamine diluted to 39 ml. with glyme. The solution is warmed to reflux and 0.2 g. of 4-dimethylaminopyridine is added. The solution is heated for four hours and cooled overnight. The solid is removed by filtration and the filtrate diluted with 200 ml. of water. The precipitate is collected and crystallized from cyclohexane. The solid is recrystallized from acetonitrile to yield the product.
WORKUP
后处理
- temperatureThe solution is warmed
- temperatureto reflux
- temperatureThe solution is heated for four hours
- temperaturecooled overnight
- customThe solid is removed by filtration
- additionthe filtrate diluted with 200 ml
- customThe precipitate is collected
- customcrystallized from cyclohexane
- customThe solid is recrystallized from acetonitrile
- customto yield the product