HRID1108604
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added in one portion
- waitset at 5° C. overnight
- extractionThis mixture was extracted three times with diethyl ether
- washThe combined extracts were washed 2 times with cold 1N hydrochloric acid
- dry with materialThe extracts were then dried over sodium sulfate/potassium carbonate
- filtrationfiltered
- concentrationconcentrated