Background and overview[1]
Bistriphenylphosphine palladium dichloride, insoluble in water. Soluble in toluene and benzene, slightly soluble in acetone and chloroform. The melting point is 260 degrees Celsius. As a catalyst, it is mainly used in coupling reactions such as Sonogoshira coupling, as a carbonylation catalyst for halides, to produce aldehydes, carboxylic acids, amides, etc. from alkyl halides, and to react with acetylene to form alkyne compounds with extended carbon chains.
Preparation[1]
Add 10g triphenylphosphorus and 45g of water into a dry one-mouth bottle, stir electromagnetically to make the system uniform; then add 3g of palladium chloride into the one-neck bottle at one time, stir and react at room temperature for 70 minutes, and observe the contents of the bottle Gradually change from black to yellow to earthy yellow until the black disappears, that is, the anti-solvent is complete. After the reaction is complete, filter and dry the filter cake under vacuum to obtain a yellow solid, which is bistriphenylphosphorus palladium dichloride. The yield is 100 %.
Apply[2-3]
Application 1,
CN201711405205.8 reports a synthesis method of L-borneol. The method includes the following steps: first, use di-n-butyltin dichloride to obtain di-n-butyltin dihydride through lithium aluminum tetrahydride reduction, and then 2-camphenone, bistriphenylphosphorus palladium dichloride, and methanol were reacted. Di-n-butyltin dihydride was added dropwise with stirring and the reaction was carried out at room temperature for 1 hour. After the reaction, the methanol was removed by rotary evaporation under reduced pressure and separated by The target compound L-borneol was obtained.
Application 2,
CN201410578910.8 reports a synthesis method of veranamine, which uses 2-bromo-5-nitroaniline as the starting material, first with 2-methyl-3-butyn-2-ol in bistriphenyl The Sonogashira coupling reaction occurs under the catalysis of phosphorus palladium dichloride and copper iodide, and then the intramolecular Michael addition cyclization reaction occurs under acidic conditions, and further Diels occurs with 3-methyl-1,2,4-triazine. -Alder reaction generates isoquinoline structural fragments. Finally, the nitro group is reduced to amino group, amino diazotization PVC composite stabilizer and bromination reaction are used to synthesize veranamine. The synthesis method of the invention is simple and has practical application prospects.
