反応 #1973314

反応方程式

di-(4-chlorobenzyl)-phenylsulfonium tetrafluoroborate

sodium hexafluoroantimonate

→

di-(4-chlorobenzyl)-benzylsulfonium hexafluoroantimonate

収率 178.1%

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.DISSOLUTIONis dissolved under N2 in a 100 ml round-bottomed flask
2. 2
   その他to give a clear solution
3. 3
   温度the solution is cooled to 0°-5° C
4. 4
   ろ過The reaction mixture is filtered
5. 5
   その他the 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
   その他the product is crystallized out
8. 8
   workup.WAITIt is left
9. 9
   その他to crystallize at 0°-5° C. for 1-2 h
10. 10
    その他The crystals now obtained by filtration
11. 11
    洗浄are washed with water
12. 12
    その他dried under a high vacuum at RT overnight

実験手順

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.

出典