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
A mixture of 13 g of benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate synthesized according to the method of JP-A 2012-107151, 14 g of bis(4-tert-butylphenyl)(4-fluorophenyl)sulfonium bromide obtained in Synthesis Example 1-3, 70 g of methylene chloride, and 30 g of deionized water was stirred for 30 minutes. The organic layer was separated, washed with water, and concentrated in vacuum. MIBK (100 g) was added to the concentrate, followed by vacuum concentration again. The residue was dissolved in methanol, after which diisopropyl ether was added for recrystallization. The resulting crystals were collected by filtration and dried in vacuum, obtaining 15 g of the target compound, bis(4-tert-butylphenyl)(4-fluorophenyl)sulfonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate as white crystals. Yield 80%.
WORKUP
后处理
- customsynthesized
- customThe organic layer was separated
- washwashed with water
- concentrationconcentrated in vacuum
- additionMIBK (100 g) was added to the concentrate
- concentrationfollowed by vacuum concentration again
- dissolutionThe residue was dissolved in methanol
- additionafter which diisopropyl ether was added for recrystallization
- filtrationThe resulting crystals were collected by filtration
- customdried in vacuum