Réaction #1840851

Équation de réaction

benzyltrimethylammonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate

bis(4-tert-butylphenyl)(4-fluorophenyl)sulfonium bromide

methylene chloride

→

target compound

Rendement 81.5%

bis(4-tert-butylphenyl)(4-fluorophenyl)-sulfonium 1,1,3,3,3-pentafluoro-2-hydroxypropane-1-sulfonate

Rendement 81.5%

Solvants

water

Conditions de réaction

Traitement

1. 1
   Autresynthesized
2. 2
   AutreThe organic layer was separated
3. 3
   Lavagewashed with water
4. 4
   Concentrationconcentrated in vacuum
5. 5
   workup.ADDITIONMIBK (100 g) was added to the concentrate
6. 6
   Concentrationfollowed by vacuum concentration again
7. 7
   workup.DISSOLUTIONThe residue was dissolved in methanol
8. 8
   workup.ADDITIONafter which diisopropyl ether was added for recrystallization
9. 9
   FiltrationThe resulting crystals were collected by filtration
10. 10
    Autredried in vacuum

Mode opératoire

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%.

Source