HRID1108604

反应详情

EQUATION

反应方程式

HRID 1108604 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

3-(4-Fluorophenoxy)propanol (7.55 g, 44 mmol) was stirred in 50 mL of pyridine under a nitrogen atmosphere at 5° C. p-Toluenesulfonyl chloride (9.2 g, 50 mmol) was added in one portion and the resulting solution was allowed to stir at 5° C. for 1 hour and then was placed in a refrigerator set at 5° C. overnight. The reaction was then poured into about 300 mL of ice water. This mixture was extracted three times with diethyl ether. The combined extracts were washed 2 times with cold 1N hydrochloric acid and once with cold water. The extracts were then dried over sodium sulfate/potassium carbonate, filtered, and concentrated to give 13.24 g of a solid product. Yield: 93%.

WORKUP

后处理

  1. additionwas added in one portion
  2. waitset at 5° C. overnight
  3. extractionThis mixture was extracted three times with diethyl ether
  4. washThe combined extracts were washed 2 times with cold 1N hydrochloric acid
  5. dry with materialThe extracts were then dried over sodium sulfate/potassium carbonate
  6. filtrationfiltered
  7. concentrationconcentrated