Background and overview[1]
Phenylmethylenebis(tricyclohexylphosphine)ruthenium dichloride is a new type of arylalkylidene-ruthenium complexes (arylalkylidene-rutheniumcomplexes), which can be used in metathesis reactions such as catalyst in.
Preparation[1-2]
Report 1,
Add 4.96 grams of benzaldehyde-p-toluenesulfonylhydrazone, 1.75 grams of sodium methoxide and 40 mL of triethylene glycol into a 100 mL single-neck bottle, and place the single-neck bottle in a water bath at 60°C. The synthesis reaction was carried out for 1 hour.
After the synthesis reaction is completed, the methanol in the obtained synthesis reaction solution is extracted with a water pump to obtain the synthesis reaction product; the synthesis reaction product is extracted with n-pentane in ice water and then saturated with NaCl aqueous solution Extract and spin the obtained extraction product to dryness to obtain phenyldiazomethane; the yield of phenyldiazomethane is 50%.
Add 4.0 grams of ruthenium tris(triphenylphosphine) dichloride into a 250 mL branch bottle, replace the air in the branch bottle with nitrogen, and inject 40 mL into the branch bottle three times. Liquid nitrogen freeze-thaw methylene chloride; place the branch bottle in a cold bath at -78°C, and add phenyldiazomethane with a mass concentration of 98.5 mg/mL at -50°C under stirring conditions 10 mL of pentane solution was mixed. The phenyldiazomethane in the pentane solution of phenyldiazomethane was the phenyldiazomethane prepared above; the resulting mixture was stirred at -70°C for 10 min and then 40 mL, A dichloromethane solution of the rubber plasticizer tricyclohexylphosphine with a mass concentration of 0.064g/mL at -50°C was reacted at 25°C for 30 minutes.
After the reaction is completed, the obtained reaction solution is filtered to remove insoluble matter. The filtered reaction solution is concentrated to 10 mL and then filtered again. To the obtained filtered product, 100 mL of liquid nitrogen freezing-thawing treatment is added to the obtained product. Precipitate with methanol, wash the obtained precipitate three times with methanol, and then wash it twice with acetone. The washed precipitate is vacuum dried for 3 hours to obtain 2.1g of the product phenylmethylene bis(tricyclohexyl). Phosphorus) ruthenium dichloride.
Report 2,
Benzylidene complex phenylmethylenebis(tricyclohexylphosphorus)ruthenium dichloride Cl2[P(C6H11)3]2Ru＝CHC6H5(3) synthesis:
Mix a suspension of 12 grams of magnesium in 100 ml of THF with 8 ml of 1,2-dichloroethane. After the violent reaction was completed, a solution of 12.2g ruthenium chloride hydrate and 42g tricyclohexylphosphane in mlTHF was added. After stirring for 10 minutes, the protective gas was replaced by hydrogen with a calculated pressure of 0.01 bar, and the solution was added in a closed The reaction mixture was heated to 60°C in the flask for 5 hours. The resulting orange suspension was cooled to -40°C, and after adding 9.7 ml of trimethylsilyl acetylene, it was heated to 5°C within 30 minutes. 1.8 ml of water were then added and the mixture was stirred at 0°C for 30 minutes. To the resulting reaction mixture was added 11.5 ml of styrene. After stirring at room temperature for 1 hour, the mixture was filtered and the filtrate was evaporated under reduced pressure. The residue was stirred with cold MeOH. The resulting purple powder was washed with cold methanol and dried under reduced pressure. Yield 37.44g (91%).
Apply[3]
CN201610733916.7 discloses a self-repairable photosensitive solder resist dry film. In the present invention, dicyclopentadiene and ethylene norbornene are first wrapped in microcapsules with a diameter of 1-10um formed by urea-formaldehyde resin. , and then combine the microcapsules with carboxyl-containing alkali-soluble polymers, vinyl-containing unsaturated monomers or oligomers, photoinitiators, auxiliaries, dicyclopentadiene, ethylene norbornene, phenyl methylene After mixing bis(tricyclohexylphosphorus)ruthenium dichloride, it is coated on the support and dried; the upper layer is bonded with a polymer covering film to obtain the self-repairable photosensitive solder resist dry film of the present invention. The invention introduces self-healing materials into the solder resist dry film, so that the solder resist dry film can realize self-repair when defects such as cracks and holes occur, thereby ensuring the solder resist and insulation of the circuit board, and to a large extent Extend the life of the circuit board.
