反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In 150 ml of dichloromethane was dissolved 42 g (0.16 mol) of the 1-octen-3-yl 2,3,3,3-tetrafluoropropionate as obtained in Reference Example 2, and the resulting solution was cooled with ice under a nitrogen atmosphere. Thereto were added 40 ml (0.2 mol) of trimethylsilyl triflate and 29 ml (0.2 mol) of triethylamine, and the resulting mixture was stirred at room temperature for 120 hours. Then, the reaction mixture was diluted with hexane, and then subjected to extraction with a 7.5% aqueous solution of sodium hydroxide. The resulting aqueous extract was acidified with concentrated hydrochloric acid, and then extracted again with dichloromethane. The resulting extract was dried with magnesium sulfate, and the solvent was removed under reduced pressure, thereby obtaining 37 g of (+)-2-fluoro-2-(trifluoromethyl)-4-decenoic acid in a yield of 88%.
WORKUP
后处理
- customas obtained in Reference Example 2
- temperaturethe resulting solution was cooled with ice under a nitrogen atmosphere
- extractionsubjected to extraction with a 7.5% aqueous solution of sodium hydroxide
- extractionThe resulting aqueous extract
- extractionextracted again with dichloromethane
- extractionThe resulting extract
- dry with materialwas dried with magnesium sulfate
- customthe solvent was removed under reduced pressure