HRID35367

反应详情

EQUATION

反应方程式

HRID 35367 的结构方程式

PROCEDURE

实验过程

Cis-4a,5,6,11b-tetrahydro-2H-[1]benzoxepino[5,4-b]-1,4-oxazine-3(4H)-one (0.01M) was added via a solution funnel to a suspension of 0.005M lithium aluminum hydride in 100 ml of dry tetrahydrofuran. The mixture was refluxed for five hours, cooled in ice and decomposed with 15% NaOH. After stirring overnight the mixture was filtered and the solvent removed from the filtrate. The residue was dissolved in ether and treated with a solution of maleic acid in ether to give the title compound. An analytical sample was recrystallized from ethyl acetate, mp. 197°-198° C. (dec.).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for five hours
  2. temperaturecooled in ice
  3. filtrationwas filtered
  4. customthe solvent removed from the filtrate
  5. dissolutionThe residue was dissolved in ether
  6. additiontreated with a solution of maleic acid in ether