A common heterocyclic compound, 680-65-9, name is Diethyl difluoromalonate, molecular formula is C7H10F2O4, 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. 680-65-9.
Step 1: Procedure for preparation of Compound 9bTo a solution of NH3/MeOH (sat., 50 mL) was added compound 9a (5 g, 25.5 mmol) at -78 C and stirred at this temperature for 2 h. Then the reaction mixture was allowed to warm to room temperature slowly and stirred overnight. The reaction mixture was concentrated under reduced pressure to dryness to give compound 9b (3.3 g, 94%) as a white solid.1H NMR (DMSO-dtf 400 MHz): delta 8.24 (br, 2H), 8.09 (br, 2H).
The synthetic route of Diethyl difluoromalonate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; DILLARD, Lawrence W.; YUAN, Jing; LEFTHERIS, Katerina; VENKATRAMAN, Shankar; WU, Guosheng; JIA, Lanqi; XU, Zhenrong; CACATIAN, Salvacion; MORALES-RAMOS, Angel; SINGH, Suresh; ZHENG, Yajun; WO2011/106414; (2011); A1;,
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