HRID1662167
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
PROCEDURE
实验过程
In 8 g of methanol was dissolved 2.1 g of triphenylsulfonium 4-benzoyloxy-1,1,2,2-tetrafluorobutanesulfonate synthesized in Synthesis Example 9. The solution was stirred under ice cooling, to which 2.5 g of a 9% sodium hydroxide aqueous solution was added dropwise at a temperature below 10° C. The solution was aged at room temperature for 70 hours, after which 22 g of 1N hydrochloric acid was added under ice cooling for quenching the reaction. The methanol was removed under vacuum. Dichloromethane was added to the organic layer, which was washed three times with water. The organic layer was concentrated and dried, obtaining the target compound. Colorless oily matter, 0.3 g.
WORKUP
后处理
- customsynthesized in Synthesis Example 9
- additionwas added dropwise at a temperature below 10° C
- customfor quenching
- customthe reaction
- customThe methanol was removed under vacuum
- additionDichloromethane was added to the organic layer, which
- washwas washed three times with water
- concentrationThe organic layer was concentrated
- customdried
- customobtaining the target compound