反応 #42148

反応方程式

tri-tert-butylphosphine sulfate

sodium tetraphenylborate

water

sodium tetraphenylborate

→

tri-tert-butylphosphonium tetraphenylborate

溶媒

toluene

反応条件

後処理

1. 1
   その他A 300-ml four-necked flask was equipped with a stirrer
2. 2
   workup.STIRRINGthe mixture was stirred at 25° C. for 3 hours
3. 3
   その他After the completion of the reaction
4. 4
   ろ過the precipitated product was filtered off
5. 5
   その他The so obtained crystal
6. 6
   ろ過filtered
7. 7
   ろ過The product filtered off
8. 8
   洗浄was washed with 100 ml of toluene
9. 9
   その他was then suspended in 100 ml of methanol at 50° C.
10. 10
    温度the suspension was cooled to 25° C.
11. 11
    ろ過filtered
12. 12
    ろ過The product filtered off
13. 13
    洗浄was washed with 100 ml of methanol
14. 14
    その他The crystal obtained
15. 15
    その他was dried

実験手順

A 300-ml four-necked flask was equipped with a stirrer, a thermometer and a reflux condenser. 16.4 g (48 mmol) of sodium tetraphenylborate and 66 ml of water were weighed in the flask, followed by stirring to dissolve sodium tetraphenylborate. While the stirring was continuously carried out, the aqueous solution of tri-tert-butylphosphine sulfate was added to the solution, and the mixture was stirred at 25° C. for 3 hours. After the completion of the reaction, the precipitated product was filtered off. The so obtained crystal was suspended in 100 ml of toluene at 50° C., and the suspension was cooled to 25° C. and filtered. The product filtered off was washed with 100 ml of toluene. The crystal was then suspended in 100 ml of methanol at 50° C., and the suspension was cooled to 25° C. and filtered. The product filtered off was washed with 100 ml of methanol. The crystal obtained was dried to give 19.4 g of objective tri-tert-butylphosphonium tetraphenylborate as white crystal. The yield (mol %) was 93% based on tri-tert-butylphosphine.

出典