HRID1596094
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
A solution of 337 mg (1 mmol) of 4,5-dibromoacridine (XIX) and 440 mg (2 mmol) of chlorodiphenylphosphane (Ph2PCl) in 40 ml of tetrahydrofuran was added dropwise to a boiling suspension of 72 mg (3 mmol) of magnesium powder in 20 ml of tetrahydrofuran. The mixture was then stirred at room temperature for 20 h. Hydrolysis with water and diluted hydrochlorid acid, extraction with diethyl ether, drying the ether phase over sodium sulfate and distilling off the solvent gave a brown raw product, from which 72 mg (15% of theory) of 4,5-bis(diphenylphosphino)acridine (Ia) was obtained as a yellow powder by several recrystallizations from dichloromethane and dichloromethane/hexane.
WORKUP
后处理
- customHydrolysis
- extractionwith water and diluted hydrochlorid acid, extraction with diethyl ether
- dry with materialdrying the ether phase over sodium sulfate
- distillationdistilling off the solvent
- customgave a brown raw product