preparation of 1,1′-bis(diphenylphosphino)ferrocene palladium dichloride ii_kain industrial additive

overview^[1]

1,1'-bis(diphenylphosphino)ferrocene palladium dichloride ii is widely used as a catalyst in the fields of organic chemistry, pharmaceutical chemistry and liquid crystal material synthesis. at present, its main synthesis methods are: 1) reaction method between palladium chloride (k, na, li salt) and dppf, 2) palladium chloride and acetonitrile (benzonitrile) complex and dppf ligand exchange method. method 1 utilizes the reaction of palladium chloride and sodium chloride (potassium chloride or lithium chloride) to obtain highly soluble chloropalladate, and then prepares 1,1'-bis(diphenylphosphino)ferrocene dichloride palladium ii, although this method shortens the reaction time and improves the reaction yield, the post-processing is cumbersome and it is easy to introduce k, na, li and other impurity ions, resulting in low quality catalyst; the acetonitrile and benzonitrile used in method 2 are both it is an extremely toxic chemical, and this method requires a long reaction time and low efficiency.

preparation^[1]

a method for preparing 1,1'-bis(diphenylphosphino)ferrocene palladium dichloride ii (dppfpdcl2), including the following steps:

(a) add palladium chloride to concentrated hydrochloric acid and heat to 40-80°c to dissolve. the amount of hydrochloric acid used is 0.2-1.0 times the mass of palladium chloride. add ethanol to dilute it. the amount of ethanol used is 10 times the mass of palladium chloride. -50 times;

(b) add 3.0-5.0 times the mass of palladium chloride of bisdiphenylphosphinoferrocene (dppf) into the tetrahydrofuran solution and heat to 40-80°c until dissolved. the amount of tetrahydrofuran used is palladium chloride. 20-30 times the mass;

(c) add the solution obtained in step (a) dropwise to the solution obtained in step (b). after the addition is completed, keep it at 45-80°c for 0.5-3h, then cool, filter, wash, and dry in vacuum. red crystals of 1,1'-bis(diphenylphosphino)ferrocene palladium ii chloride were obtained.

main reference materials

[1] cn201210279150.1 preparation method of [1,1''-bis(diphenylphosphino)ferrocene]palladium dichloride