Catalyst, preparation method thereof and preparation method of amide compound
A technology of amide compounds and catalysts, applied in the field of catalyst preparation, which can solve the problems of restricting large-scale applications, large catalyst usage, and narrow substrate application range
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[0059] see figure 1 , the preparation method of the catalyst of one embodiment, comprises the following steps:
[0060] S110, reacting the precursor and the first ligand in the first solvent at 20° C. to 80° C. to obtain an intermediate.
[0061] In one embodiment, the step of mixing the precursor and the first ligand in the first solvent at 20°C to 80°C to obtain the intermediate specifically includes:
[0062] S111. Dissolving the precursor and the first ligand in the first solvent and mixing them at 20° C. to 80° C. to obtain a first reaction solution.
[0063] In one embodiment, the precursor is selected from at least one of (1,5-cyclooctadiene)platinum chloride and (1,5-cyclooctadiene)platinum bromide.
[0064] In one of the embodiments, the first ligand is selected from 1,1'-bis(diphenylphosphino)ferrocene, 1,1'-bis[(5-methyl-2-furyl)phosphino] Ferrocene, (-)-1,1-bis((2S,4S)-2,4-diethylphosphino)ferrocene, (-)-1,1-bis((2S,5S)-2 ,4-Dimethylphosphino)ferrocene, (1R)-1[...
Embodiment 1
[0121] The preparation method of the catalyst of the present embodiment is as follows:
[0122] Dissolve (1,5-cyclooctadiene)platinum chloride and 1,1'-bis(diphenylphosphino)ferrocene in dichloromethane at a molar ratio of 1:1, and then proceed at 25°C Stirring for 12 hours to obtain the first reaction solution, filtering the first reaction solution to obtain a filtrate, and distilling the filtrate under reduced pressure to obtain a solid, dissolving the solid in dichloromethane, then adding n-hexane to it for recrystallization to obtain an intermediate, The volume ratio of dichloromethane to n-hexane is 1:1; the intermediate obtained above, dimethyl hydroxyphosphine and silver tetrafluoroborate are dissolved in dichloromethane, and then stirred at 25°C for 12h to obtain the second reaction liquid, wherein the molar ratio of the intermediate to dimethylhydroxyphosphorus is 1:1.05, and the molar ratio of the intermediate to silver tetrafluoroborate is 1:1; the second reaction l...
Embodiment 2
[0132] The preparation method of the catalyst of the present embodiment is as follows:
[0133] Dissolve (1,5-cyclooctadiene)platinum chloride and 1,1'-bis[(5-methyl-2-furyl)phosphino]ferrocene in dichloro In methane, stirred at 40°C for 4h to obtain the first reaction solution, filtered the first reaction solution to obtain a filtrate, and distilled the filtrate under reduced pressure to obtain a solid, dissolved the solid in dichloromethane, and then added N-hexane is recrystallized to obtain an intermediate, and the volume ratio of dichloromethane to n-hexane is 1:1; the intermediate obtained above, dimethyl hydroxyphosphine and silver trifluoromethanesulfonate are dissolved in dichloromethane, and then Stir at 40°C for 4h to obtain a second reaction solution, wherein the molar ratio of the intermediate to dimethylhydroxyphosphorus is 1:1.05, and the molar ratio of the intermediate to silver tetrafluoroborate is 1:1; the second reaction Liquid is filtered to obtain filtrat...
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