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
5.5 g of 1-methyl-5-hydroxy-8-benzyloxy-3,4-dihydrocarbostyril was added to 15 g of epichlorohydrin, and 12 drops of piperidine were then added thereto followed by stirring at 90° to 100° C. for 3 hours. The unreacted epichlorohydrin and piperidine were evaporated under reduced pressure, and the residue was dissolved in chloroform, washed successively with a 5% aqueous solution of sodium hydroxide and water and dried over anhydrous potassium carbonate. The chloroform was evaporated under reduced pressure, and the residue was purified by silica gel chromatography and then recrystallized from ethanol to afford 3.5 g of 1-methyl-5-(2,3-epoxypropoxy)-8-benzyloxy-3,4-dihydrocarbostyril as yellow needle-like crystals having a melting point of 111°-112.5° C.
WORKUP
后处理
- additionwere then added
- customThe unreacted epichlorohydrin and piperidine were evaporated under reduced pressure
- dissolutionthe residue was dissolved in chloroform
- washwashed successively with a 5% aqueous solution of sodium hydroxide and water
- dry with materialdried over anhydrous potassium carbonate
- customThe chloroform was evaporated under reduced pressure
- customthe residue was purified by silica gel chromatography
- customrecrystallized from ethanol