HRID1155571

反应详情

EQUATION

反应方程式

HRID 1155571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwere then added
  2. customThe unreacted epichlorohydrin and piperidine were evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in chloroform
  4. washwashed successively with a 5% aqueous solution of sodium hydroxide and water
  5. dry with materialdried over anhydrous potassium carbonate
  6. customThe chloroform was evaporated under reduced pressure
  7. customthe residue was purified by silica gel chromatography
  8. customrecrystallized from ethanol