HRID638059

反应详情

EQUATION

反应方程式

HRID 638059 的结构方程式

PROCEDURE

实验过程

0.5 g of 2-(4-hydroxyphenyl)-thiazole is added in one portion to a mixture, heated under reflux, of 5 ml of epichlorohydrin and 0.79 g of potassium carbonate and the reaction mixture is then heated under reflux for a further 20 minutes. After cooling, the mixture is filtered, the filtrate is concentrated by evaporation in a rotary evaporator and the residue is dissolved in 6 ml of dichloromethane; 100 mg of tetrabutylammonium hydrogen sulphate and 6 ml of 2N sodium hydroxide solution are added to the solution and the whole is stirred for 3 hours at room temperature. The organic phase is separated off, washed with water and dried over sodium sulphate and the solvent is then removed in a rotary evaporator. The residue is recrystallised from a mixture of ether/hexane, yielding 2-[4-(2,3-epoxypropoxy)-phenyl]-thiazole having a melting point of 82°-93°.

WORKUP

后处理

  1. temperatureheated
  2. temperaturethe reaction mixture is then heated
  3. temperatureunder reflux for a further 20 minutes
  4. temperatureAfter cooling
  5. filtrationthe mixture is filtered
  6. concentrationthe filtrate is concentrated by evaporation in a rotary evaporator
  7. dissolutionthe residue is dissolved in 6 ml of dichloromethane
  8. addition100 mg of tetrabutylammonium hydrogen sulphate and 6 ml of 2N sodium hydroxide solution are added to the solution
  9. customThe organic phase is separated off
  10. washwashed with water
  11. dry with materialdried over sodium sulphate
  12. customthe solvent is then removed in a rotary evaporator
  13. customThe residue is recrystallised from a mixture of ether/hexane