Electric Literature of 680-65-9,Some common heterocyclic compound, 680-65-9, name is Diethyl difluoromalonate, molecular formula is C7H10F2O4, 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.
In a dry 25 mL round bottom flask under an Ar atmosphere, NaOEt (9.71 mL, 26.0mmol) in EtOH (21 % weight) and diethyl-2,2-difluoromalonate (2.55 g, 13.0 mmol) werestirred at rt for 10 mm. A solution of Example id (554 mg, 1.30 mmol) in EtOH (6.00mL) was added dropwise and the reaction was stirred at rt over 18 hrs. The EtOH wasremoved in vacuo and the crude oil was dissolved in 1 M HC1 (10 mL). The aqueoussolution was extracted with EtOAc (20 mL x 3), and the combined organics were washedwith aq NaC1 (20 mL), dried over Na2SO4, filtered into a round bottom flask andconcentrated in vacuo to give the title compound as a crude brown oil (749 mg, 1.30mmol). MS (ESI) 576.0 [M+H]+.
The synthetic route of 680-65-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; EXELIXIS PATENT COMPANY LLC; KICK, Ellen, K.; BODAS, Mandar; MOHAN, Raju; BUSCH, Brett, B.; AVERBUJ, Claudia; VALENTE, Meriah; WURTZ, Nicholas; RAO, Prasanna Savanor, Maddu; SHETTY, Jeevanprakash; VENU, Alla; WO2014/152738; (2014); A1;,
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