反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a suspension of 43.6 grams of diphenylphosphinic acid in 300 milliliters of distilled water is added a solution of 8.0 grams of sodium hydroxide in 200 milliliters of water and the mixture stirred. The acid dissolves slowly. To the resulting solution is added a solution of 59 grams of tetra-n-butylphosphonium chloride in about 200 milliliters of distilled water. The reaction mixture is stirred for half an hour and is then extracted with two 250-milliliter portions of chloroform. The extract is dried over anhydrous Na2SO4 and the chloroform is then distilled. A light-brown viscous liquid remains. It is dried overnight at 80° C. On cooling, tetra-n-butylphosphonium diphenylphosphinate separates as white crystals. It is collected by filtration and is washed with anhydrous ether; the crystals melt at 83° to 84° C.
WORKUP
后处理
- dissolutionThe acid dissolves slowly
- stirringThe reaction mixture is stirred for half an hour
- extractionis then extracted with two 250-milliliter portions of chloroform
- dry with materialThe extract is dried over anhydrous Na2SO4
- distillationthe chloroform is then distilled
- customIt is dried overnight at 80° C
- temperatureOn cooling
- filtrationIt is collected by filtration
- washis washed with anhydrous ether
- custommelt at 83° to 84° C.