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
Bis(4-tert-butylphenyl)iodonium hydrogen sulfate (0.02 mole equivalent) prepared in Synthesis Example 1-6, 0.024 mole equivalent of the aqueous solution of sodium 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropane-1-sulfonate prepared in Synthesis Example 1-9, and 70 g of methylene chloride were mixed and agitated at room temperature for 1 hour. After the agitation, the organic layer was separated, washed by water, and then concentrated under reduced pressure. The residue was recrystallized by adding diisopropyl ether, and then the obtained crystals were recovered and dried to obtain the intended bis(4-tert-butylphenyl)iodonium 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropane-1-sulfonate (9.4 g of white crystals (yield 72%)). The structure of the intended product is shown below.
WORKUP
后处理
- additionwere mixed
- customAfter the agitation, the organic layer was separated
- washwashed by water
- concentrationconcentrated under reduced pressure
- customThe residue was recrystallized
- additionby adding diisopropyl ether
- customthe obtained crystals were recovered
- customdried