HRID653515

反应详情

EQUATION

反应方程式

HRID 653515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of sodium 3,4-dihydro-2H-pyran-2-carboxylate (150.0 g, 10 mol), ethyl iodide (192.3 g, 1.2 mol), sodium carbonate (10 g), and dimethylformamide (500 ml) was heated at 105°-110° C. for 5 hours. The reaction mixture was cooled to room temperature and water (450 ml) was added to dissolve inorganic sales. The mixture was extracted with four 200 ml portions of benzene. The combined organic layers were washed with four 200 ml portions of water and dried over anhydrous magnesium sulfate. The solution was filtered and the solvent was removed by rotary evaporation. The oily residue was distilled under reduced pressure giving a yield of 87% of product having a bp of 75°-80° C.

WORKUP

后处理

  1. temperaturewas heated at 105°-110° C. for 5 hours
  2. dissolutionto dissolve inorganic sales
  3. extractionThe mixture was extracted with four 200 ml portions of benzene
  4. washThe combined organic layers were washed with four 200 ml portions of water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationThe solution was filtered
  7. customthe solvent was removed by rotary evaporation
  8. distillationThe oily residue was distilled under reduced pressure