HRID1595062

反应详情

EQUATION

反应方程式

HRID 1595062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4′-(2-Hydroxy ethyl)octanophenone (1.0 g) prepared in the step B was dissolved in dichloromethane (10 ml) to obtain a solution. p-Toluene sulfonyl chloride (923 mg) and pyridine (383 mg) were added to the solution with cooling, and the mixture was stirred at room temperature for 2 hours. After the reaction, ice water was added to the solution, the solution was stirred at room temperature for 20 minutes. Dichloromethane layer was washed with 2% hydrochloric acid, sodium bicarbonate solution, and water. The dichloromethane layer was dried over anhydrous sodium sulfate, and concentrated. The residue was recrystallized from hexane-ethyl acetate (10:1) to obtain 2-(4-octanoyl phenyl)ethyl p-toluene sulfonate (950 mg) in the form of colorless crystal.

WORKUP

后处理

  1. customto obtain a solution
  2. temperaturewith cooling
  3. additionwas added to the solution
  4. stirringthe solution was stirred at room temperature for 20 minutes
  5. washDichloromethane layer was washed with 2% hydrochloric acid, sodium bicarbonate solution, and water
  6. dry with materialThe dichloromethane layer was dried over anhydrous sodium sulfate
  7. concentrationconcentrated
  8. customThe residue was recrystallized from hexane-ethyl acetate (10:1)