反応 #1973310

反応方程式

charcoal

sodium hexafluoroantimonate

tribenzylsulfonium hydrogen sulfate

→

tribenzylsulfonium hexafluoroantimonate

収率 74.0%

溶媒

methanol

反応条件

後処理

1. 1
   ろ過the mixture is filtered
2. 2
   workup.ADDITION750 ml of water are added to the clear filtrate
3. 3
   その他The crystals which have precipitated
4. 4
   ろ過are filtered off
5. 5
   その他dried
6. 6
   洗浄washed with 100 ml of ether
7. 7
   その他dried again

実験手順

16.64 g (0.041 mol) of tribenzylsulfonium hydrogen sulfate are dissolved in 750 ml of hot methanol. 16.04 g (0.062 mol) of solid sodium hexafluoroantimonate are added to the cloudy solution and the mixture is stirred at RT for 1 h. After addition of 1 spatula-full of active charcoal, the mixture is filtered and 750 ml of water are added to the clear filtrate. The crystals which have precipitated are filtered off, dried, washed with 100 ml of ether and dried again. 16.41 g (74% of theory) of tribenzylsulfonium hexafluoroantimonate are obtained as colourless crystals of melting point 170° C. (decomposition).

出典