Application of 2687-12-9, These common heterocyclic compound, 2687-12-9, name is Cinnamyl chloride, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A)In a two-necked flask equipped with a magnetic stirrer,250 mL of distilled water was added and argon was bubbled in for 30 minutes;B)Continue to maintain through the argon gas flow,PdCI2 (10 mmol, 1.77 g, 1 equiv) and KCl (2.84 g,4equiv),And then sealed with a rubber stopper to the mouth of the flask,The mixture in the flask was stirred for 1 hour;C)The excess of cinnamyl chloride (Ph-allyl) Cl (4.58 g, 3 equiv) was injected into the reaction flask through a rubber stopper,The resulting system continued to react for 24 hours;D)The reaction mixture was extracted three times with chloroform,The organic phases were combined,Dried over anhydrous MgSO4, filtered, the solvent removed under reduced pressure,To obtain the corresponding dimer;E)N- [2-bis (1-adamantyl) phosphophenyl] morpholine (2.2 mmol, 1.02 g) and 15 mL of dry tetrahydrofuran (THF) were charged in a single jar equipped with a magnetic stirrer,1 mmol of the above-mentioned palladium dimer was added to dissolve the ligand,Close the lid,The mixture was stirred at room temperature for 3 hours;F)The solvent was then removed under reduced pressure,A solid was obtained.The solid was pulverized in pentane,Filtered and recrystallized from 10 mL of dichloromethane (DCM) / pentane (1: 1 weight ratio)dry,Pulverization can be obtained palladium complex catalyst 2.37g.
The synthetic route of 2687-12-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shandong Chuancheng Pharmaceutical Co., Ltd.; Liu, Huaizhen; Guo, Ming; Ma, Juliang; (6 pag.)CN106083599; (2016); A;,
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