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
- 40 °C
PROCEDURE
实验过程
Using the 2,2-bis(trifluoromethyl)oxirane prepared in Synthesis Example 1-2, synthesis was carried out in accordance with the procedure described in US 20100209827. A mixture of 30 g of 2,2-bis(trifluoromethyl)oxirane, 26 g of sodium hydrogensulfite, and 120 g of water was stirred at 40° C. for 10 hours, obtaining an aqueous solution of sodium 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropane-1-sulfonate. Subsequently, 34 g of an aqueous solution of 2,000 g/mol of triphenylsulfonium chloride and 400 g of methylene chloride were added to the aqueous solution, which was stirred for 4 hours at room temperature. At the end of stirring, the organic layer was taken out, washed with water, and concentrated under reduced pressure. The concentrate was combined with methyl isobutyl ketone and concentrated again under reduced pressure to distill off the residual water. To the residue, diisopropyl ether was added for recrystallization, obtaining 74 g of triphenylsulfonium 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropane-1-sulfonate (yield 85%).
WORKUP
后处理
- customprepared in Synthesis Example 1-2, synthesis