HRID462042

反应详情

EQUATION

反应方程式

HRID 462042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.23 g of sodium metal was dissolved in 40 ml of methanol, and 2.53 g of 1-benzyl-5-hydroxy-3,4-dihydrocarbostyril and 1.3 g of glycerol α-monochlorohydrin were added to the resulting solution followed by refluxing the mixture for 6 hours. After allowing the mixture to cool, the precipitated crystals were filtered, and the filtrate was concentrated to dryness. The residue thus obtained was extracted with 50 ml of chloroform, and the extract was washed with a 5% aqueous sodium hydroxide solution and then water and then dried over anhydrous sodium sulfate. The chloroform was then removed by distillation and the resulting residue was recrystallized from ethanol to give 1.2 g of 1-benzyl-5-(2,3-dihydroxy)propoxy-3,4-dihydrocarbostyril as a colorless amorphous solid having a melting point of 153° - 155° C.

WORKUP

后处理

  1. temperatureby refluxing the mixture for 6 hours
  2. temperatureto cool
  3. filtrationthe precipitated crystals were filtered
  4. concentrationthe filtrate was concentrated to dryness
  5. customThe residue thus obtained
  6. extractionwas extracted with 50 ml of chloroform
  7. washthe extract was washed with a 5% aqueous sodium hydroxide solution
  8. dry with materialwater and then dried over anhydrous sodium sulfate
  9. customThe chloroform was then removed by distillation
  10. customthe resulting residue was recrystallized from ethanol