Reaction #1973314

Reaction equation

di-(4-chlorobenzyl)-phenylsulfonium tetrafluoroborate

sodium hexafluoroantimonate

→

di-(4-chlorobenzyl)-benzylsulfonium hexafluoroantimonate

Yield 178.1%

Solvents

methylene chloride

Conditions

Workup

1. 1
   workup.DISSOLUTIONis dissolved under N2 in a 100 ml round-bottomed flask
2. 2
   Otherto give a clear solution
3. 3
   Temperaturethe solution is cooled to 0°-5° C
4. 4
   FiltrationThe reaction mixture is filtered
5. 5
   Otherthe filtrate is freed from the solvent on a rotary evaporator
6. 6
   workup.ADDITION50 ml of deionized water are now added to the residue
7. 7
   Otherthe product is crystallized out
8. 8
   workup.WAITIt is left
9. 9
   Otherto crystallize at 0°-5° C. for 1-2 h
10. 10
    OtherThe crystals now obtained by filtration
11. 11
    Washare washed with water
12. 12
    Otherdried under a high vacuum at RT overnight

Procedure

A mixture of 7.0 g (15.2 mmol) of di-(4-chlorobenzyl)-phenylsulfonium tetrafluoroborate and 25 ml of methylene chloride is dissolved under N2 in a 100 ml round-bottomed flask to give a clear solution and the solution is cooled to 0°-5° C. 5.9 g (22.8 mmol) of sodium hexafluoroantimonate are added at this temperature and the mixture is stirred for about 3 h. The reaction mixture is filtered and the filtrate is freed from the solvent on a rotary evaporator. 50 ml of deionized water are now added to the residue and the product is crystallized out. It is left to crystallize at 0°-5° C. for 1-2 h. The crystals now obtained by filtration are washed with water and dried under a high vacuum at RT overnight. 8.26 g of di-(4-chlorobenzyl)-benzylsulfonium hexafluoroantimonate are obtained as white crystals of melting point 75°-77° C.

Source