HRID132738

反应详情

EQUATION

反应方程式

HRID 132738 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 0.1 mol sodium hydride was added 100 ml anhydrous tetrahydrofuran, then added slowly dropwise 0.1 mol 6-methyl-2,4-heptandione at room temperature. The reaction was stirred for 0.5 hours, then 0.12 mol iodomethane was added dropwise and the reaction was stirred at room temperature for further 10 hours. Upon completing the reaction, 20 ml water was added. The mixture was extracted with ethyl acetate. After removing the solvent, distillation under reduced pressure gave a cut fraction 88-9° C./1 kPa (165-166° C. at atmosphere pressure), and the yield was 94%.

WORKUP

后处理

  1. stirringthe reaction was stirred at room temperature for further 10 hours
  2. additionwas added
  3. extractionThe mixture was extracted with ethyl acetate
  4. customAfter removing
  5. distillationthe solvent, distillation under reduced pressure
  6. customgave a cut fraction 88-9° C./1 kPa (165-166° C. at atmosphere pressure)