HRID329828

反应详情

EQUATION

反应方程式

HRID 329828 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 10.0 g of water was dissolved 10.0 g of tri-n-butylmethylphosphonium carbonate and 7.9 g of an aqueous solution of 42% HBF4 was gradually added to the solution, whereby carbon dioxide simultaneously generated vigorously. For more completely removing carbon dioxide from the system, degassing was performed for 2 hours at 40° C. and 20 mmHg and after confirming carbon dioxide being less than 20 ppm, water was distilled off. The residue formed was recrystallized from a mixture of water and methanol to provide 10.1 g (92.4% of the theoretical yield, yield of 58.8% to tri-n-butylphosphine) of tri-n-butylmethylphosphonium tetrafluoroborate.

WORKUP

后处理

  1. customFor more completely removing carbon dioxide from the system, degassing
  2. distillationwas distilled off
  3. customThe residue formed
  4. customwas recrystallized from a mixture of water and methanol