Application of lj reaction in palladium-catalyzed cross-coupling reaction
A reaction and compound technology, applied in the application field of LJ reaction in palladium-catalyzed cross-coupling reaction, can solve the problems that are not suitable for large-scale and large-scale industrial production
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Embodiment 1
[0037] Embodiment 1 molecular ratio: sodium phenate: PCl 5 : phenyllithium = 1:1:1
[0038] Under the condition of isolating air and water, 40 grams of PCl 5 with 200 g CCl 4 Put it into the reactor, start stirring, control the temperature below -15°C, slowly add the calculated amount of sodium phenate, and keep it warm for about 1 hour. During the process, the generated NaCl is continuously filtered out through the external circulation, and 13 compounds are generated at this time , yield 98%.
[0039] Throw calculated amount of benzene, AlCl 3 and 120 g CCl 4 into the reaction flask, start stirring, control the temperature to reflux, drop cold insulation 13 compound CCl 4 Solution, after dripping, keep warm for 1 hour, during the process, continuously distill the by-product phosphorus oxychloride azeotropically, and add CCl continuously at the same time 4 Solvent, after reacting to the end point, distill off CCl 4 , add 400 grams of 70% aqueous methanol for extraction,...
Embodiment 2
[0040] Embodiment 2 Molecular ratio: 20 compounds: PCl 5 : lithium o-toluene = 1:2:1
[0041] Under nitrogen protection, 40 g of PCl 5 with 200 g CCl 4 Put the solution into the reactor, start stirring, control the temperature below 20°C, add the calculated amount of the mixed solution of 20 compounds and o-toluene lithium dropwise, and keep the reaction for 11 hours. During the process, the LiCl solid generated simultaneously is continuously filtered out through the external circulation, and then Raise the temperature to reflux, and after the reaction reaches the end point, slowly distill off the phosphorus oxychloride, then raise the temperature to 160-170°C, and add PCl 5 After sublimation, recover and use mechanically, cool down, and wash the remaining PCl with 5% NaOH alkaline water 5 , plus 200 g CCl 4 Dissolving and extracting, separating layers, collecting the organic layer for distillation, lowering the temperature, standing still, crystallizing, filtering and dry...
Embodiment 3
[0043] Molecular ratio: 21 compounds: triphenylphosphine dichloride: alkyl lithium = 1:1:1
[0044]Under the condition of isolating air and water, put 40 grams of triphenylphosphine dichloride and 280 grams of n-hexane into the reactor, start stirring, control the temperature below -5°C, slowly add the calculated amount of compound 21, and keep warm for the reaction 1 hour, during the process, the generated LiCl was continuously filtered out through the external circulation, and 18 compounds were generated at this time, with a yield of 98%;
[0045] Put the calculated amount of o-methyllithium and 120 grams of n-hexane into the reactor, start stirring, control the temperature and reflux, add dropwise the 18 compound n-hexane solution of cold insulation, after the drop, keep the temperature for 1 hour, during the process, through the external circulation The generated lithium chloride solid was continuously filtered out, and after the reaction reached the end point, the solvent...
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