With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.13031-04-4,4,4-Dimethyldihydrofuran-2,3-dione,as a common compound, the synthetic route is as follows.,13031-04-4
A rhodium catalyst precursor [Rh(COD)Cl]2, a chiral bisphosphine ligand 3 (R1 = Boc), a polyether alkylguanidinium salt ionic liquid [ (PG), CH3 (EO) 16TMG] SO3CH3, ketopantolactone and benzene, the molar ratio of 3 to Rh is 1.1: 1, the mass ratio of ionic liquid to rhodium catalyst precursor is 500: 1, the ratio of ketopantolactone to Rh The molar ratio is 100: 1, the volume ratio of benzene to ionic liquid is 4: 1, the atmosphere is replaced with nitrogen or argon for 4-6 times, and then pressurized with hydrogen to 5.0MPa, the reaction is carried out at 50 for 4 hours and then rapidly cooled After hydrogen was vented, the benzene was removed under reduced pressure and extracted twice with methyl tert-butyl ether. The volume ratio of methyl tert-butyl ether to benzene was 1: 1. The system was split into two phases and was isolated by simple phase separation The upper methyl tert-butyl ether phase containing D-pantolactone was analyzed by gas chromatography. The conversion of ketopantolactone was 77.6%, and the ee value of D-pantolactone was 60.7%. The reaction conditions and procedures were the same as in Example 1 except that the solvent was changed to toluene, the molar ratio of ketopantolactone to Rh was 200: 1, the pressure of hydrogen was 0.1 MPa, the reaction temperature was 25 C, and the reaction time was 2h. Analysis by gas chromatography showed that the conversion rate of ketopantolactone was 97.5% and that of D-pantolactone was 92.2%.
The synthetic route of 13031-04-4 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; Qingdao University of Science and Technology; Jin Xin; Li Shumei; Cui Feifei; (8 pag.)CN104761518; (2017); B;,
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