With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.10521-08-1,2H-Pyran-2,4,6(3H,5H)-trione,as a common compound, the synthetic route is as follows.,10521-08-1
To a 3 L flask with 53.6 g (0.41 mol) of 2,5-dimethoxydihydrofuran was added 1000 ml of 3N HCl solution.. The mixture was left to stand for 12 h at room temperature and then neutralized with ice-cold NaOH solution (equal moles) at 0 C. To this red solution, was added 41.3 g (0.62 mol) of methylamine hydrochloride in 300 ml H2O, the preformed methanol solution of the monomethylester (50 g (0.39 mol) of acetone dicarboxylic acid anhydride in 160 ml of methanol) and 50 g of sodium acetate in 200 ML of H2O. The mixture (PH 4.5) was stirred for 2 days and the acidity decreased to PH 4.9.. The red solution was extracted with hexane (450 ml*2) to remove nonpolar by-products.. The aqueous solution was basified first with NaOH (1N) to neutral PH, then with potassium carbonate.. sodium chloride (about 200 g) was added.. The saturated solution was extracted with CH2Cl2 (250 ml*8), then with a mixed solvent (t-butyl:1,2-dichloroethane, 37:63, 250 ml*8).. The CH2Cl2 extracted was dried over K2CO3 and solvent was removed to provide 19.6 g of a crude mixture which was separated by column chromatography (SiO2, 10% Et3N, 30-90% EtOAc in hexane and 10% methanol in EtOAc) to afford 7.5 g of 6(7)-methoxy-2-methoxycarbonyl-8-azabicyclo(3.2.1)octane-2-one as an oil and 7 g of 6(7)-hydroxy-2-methoxycarbonyl-8-azabicyclo-(3.2.1)octane-2-one as a crystalline solid.
The synthetic route of 10521-08-1 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; Organix, Inc.; President and Fellows of Harvard College; US6353105; (2002); B1;,
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