HRID1728512

反应详情

EQUATION

反应方程式

HRID 1728512 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

17 g of 2-fluorodecanol and 60 ml of pyridine were charged into a 300 ml three-necked round bottom flask and cooled to 0° C. to which 24 g of p-toluenesulfonyl chloride was added in 15 min. The system was held at 0° C. for 1 hour and then subjected to reaction for 7 hours while being held below 20° C. Then, the mixture was charged into water and acidified with hydrochloric acid, followed by extraction with dichloromethane. The organic layer was washed with water, dried with magnesium sulfate and then purified by silica gel chromatography with the use of dichloromethane as the eluent to obtain 23 g of 2-fluorodecyl p-toluenesulfonate.

WORKUP

后处理

  1. additionwas added in 15 min
  2. customsubjected to reaction for 7 hours
  3. customwhile being held below 20° C
  4. extractionfollowed by extraction with dichloromethane
  5. washThe organic layer was washed with water
  6. dry with materialdried with magnesium sulfate
  7. custompurified by silica gel chromatography with the use of dichloromethane as the eluent