Synthetic Route of 6065-54-9, These common heterocyclic compound, 6065-54-9, name is Dimethyl 2,2-dimethylmalonate, 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.
Step 2: 2.63 g Mg in 75 ml anhydrous THF are preheated to 55C, treated with 20 mg iodine and 20 mg methyl iodide, 25.7 g of 5-bromo-7-methoxy-2,2-dimethyl-2,3-dihydro-1-benzofuran (see below) are added maintaining reflux of the reaction, and the reaction is heated to reflux for 3 h until most of the Mg disappeared. 20 g dimethyl dimethylmalonate are solved in 40 ml anhydrous THF, cooled to – 6OC, and the freshly prepared Grignard reagent is added drop wise over 1 h at this temperature. The reaction is allowed to warm to 5C and quenched with 250 ml saturated aqueous ammonium chloride solution. The reaction is extracted with ether twice, the combined organic layers are dried over MgSO4, and the solvent is removed under reduced pressure. The crude product may contain some unreacted dimethyl dimethylmalonate, which could largely be distilled off under vacuum. The crude product is used for the cyclisation reaction without further purification.;
Statistics shows that Dimethyl 2,2-dimethylmalonate is playing an increasingly important role. we look forward to future research findings about 6065-54-9.
Reference:
Patent; NYCOMED GMBH; SCHLEMMINGER, Imre; SCHMIDT, Beate; FLOCKERZI, Dieter; TENOR, Hermann; ZITT, Christof; HATZELMANN, Armin; MARX, Degenhard; BRAUN, Clemens; KUeLZER, Raimund; HEUSER, Anke; KLEY, Hans-Peter; STERK, Geert Jan; WO2010/55083; (2010); A1;,
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