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
CONDITIONS
反应条件
- 温度
- 23 °C
PROCEDURE
实验过程
8.70 g (2127.5 mmol) of NaOH in 40 ml of water were added dropwise at 23° C. to a solution of 34.52 g (87 mmol) of isobutyl (4-diphenylphosphino-phenyl)methylphosphinate in 50 ml of THF. After heating under reflux for 6 hours, 18.1 ml (218 mmol) of concentrated hydrochloric acid were added dropwise at 23° C., the mixture was stirred for 10 minutes at 23° C. and completely evaporated on a rotary evaporator. The residue is taken up in methylene chloride, the solution was dried over Na2SO4 and completely evaporated. Drying under reduced pressure gave 28.3 g of (4-diphenylphosphinophenyl)methylphosphinic acid (90% of theory) in the form of a pale yellow solid having a melting point of 40° C.
WORKUP
后处理
- temperatureAfter heating
- temperatureunder reflux for 6 hours
- customcompletely evaporated on a rotary evaporator
- dry with materialthe solution was dried over Na2SO4
- customcompletely evaporated
- customDrying under reduced pressure