HRID1744719

反应详情

EQUATION

反应方程式

HRID 1744719 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 500 niL round bottom flask equipped with a mechanical stirrer was charged with 16.7g (0.15 mol) 2-butoxyethanol, and 150 mL of DMSO. Sodium hydride (4.22 g, 95% in purity; 0.167 mol) was slowly added to above mixture in an ice bath over 20 min. After the above mixture was reacted at room temperature for 3 hrs, 39.9 g (0.15 mol) of 3-cyclohexene-1-methanol tosylate was slowly added to the above mixture over 20 min. The reaction was carried at room temperature overnight, then 80° C. for 3 hrs. The reaction mixture was added to water (150 mL), and then extracted with chloroform (3×150 mL), washed with water (2×100 mL), dried with sodium sulfate. The solvent was evaporated and the residue distilled to give pure product.

WORKUP

后处理

  1. customA 500 niL round bottom flask equipped with a mechanical stirrer
  2. customAfter the above mixture was reacted at room temperature for 3 hrs
  3. wait80° C. for 3 hrs
  4. extractionextracted with chloroform (3×150 mL)
  5. washwashed with water (2×100 mL)
  6. dry with materialdried with sodium sulfate
  7. customThe solvent was evaporated
  8. distillationthe residue distilled
  9. customto give pure product