HRID486346

反应详情

EQUATION

反应方程式

HRID 486346 的结构方程式

PROCEDURE

实验过程

In a vessel sufficiently replaced with nitrogen, 0.40 g (3.0 mmol) of (-)-2-fluoroheptanol and 1.00 g (13 mmol) of dry pyridine were placed and dried for 30 min. under cooling on an ice bath. Into the solution, 0.69 g (3.6 mmol) of p-toluenesulfonyl chloride was added, and the mixture was stirred for 5 hours. After the reaction, 10 ml of 1N-HCl was added, and the resultant mixture was subjected to two times of extraction with 10 ml of methylene chloride. The extract liquid was washed once with 10 ml of distilled water and dried with an appropriate amount of anhydrous sodium sulfate, followed by distilling-off of the solvent to obtain 0.59 g (2.0 mmol) of (+)-2-fluoroheptyl p-toluenesulfonate.

WORKUP

后处理

  1. customdried for 30 min.
  2. temperatureunder cooling on an ice bath
  3. additionwas added
  4. extractionthe resultant mixture was subjected to two times of extraction with 10 ml of methylene chloride
  5. washThe extract liquid was washed once with 10 ml of distilled water
  6. dry with materialdried with an appropriate amount of anhydrous sodium sulfate