反応 #1973312

反応方程式

dibenzylsulfonium tetrafluoroborate

sodium hexafluoroantimonate

→

dibenzylphenylsulfonium hexafluoroantimonate

収率 191.3%

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.DISSOLUTIONis dissolved in a 2 liter round-bottomed flask at RT under N2
2. 2
   その他to give a clear solution
3. 3
   ろ過The suspension is now filtered over silica gel
4. 4
   その他the solvent is removed from the filtrate
5. 5
   その他a rotary evaporator
6. 6
   workup.DISSOLUTIONThe slightly reddish viscous residue is dissolved again in 250 ml of methanol
7. 7
   workup.ADDITIONafter addition of 250 ml of water the product
8. 8
   その他to crystallize at RT for 1-2 h
9. 9
   ろ過The suspension is filtered
10. 10
    洗浄the residue is washed with water
11. 11
    その他The product is then dried under a high vacuum at RT overnight

実験手順

A mixture of 123.0 g (0.325 mol) of dibenzylsulfonium tetrafluoroborate in 400 ml of methylene chloride is dissolved in a 2 liter round-bottomed flask at RT under N2 to give a clear solution. 117.8 g of sodium hexafluoroantimonate are then added and the mixture is stirred at RT for 31/2 h. The suspension is now filtered over silica gel and the solvent is removed from the filtrate using a rotary evaporator. The slightly reddish viscous residue is dissolved again in 250 ml of methanol, and after addition of 250 ml of water the product is allowed to crystallize at RT for 1-2 h. The suspension is filtered and the residue is washed with water. The product is then dried under a high vacuum at RT overnight. 163.9 g (95% of theory) of dibenzylphenylsulfonium hexafluoroantimonate are obtained as white crystals of melting point 105°-109° C.

出典