Reference of 681128-38-1,Some common heterocyclic compound, 681128-38-1, name is Ethyl 3,3-difluorocyclobutanecarboxylate, molecular formula is C7H10F2O2, 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.
A solution of the compound described in Preparation 42 (2.30 g, 14 mmol), in diethyl ether (14 ml_), was added to a suspension of lithium aluminium hydride (1.17 g, 30.8 mmol), in diethyl ether (70 ml_), cooled to -45 0C. This mixture was stirred at -45 0C for 1 hour, then warmed to -10 0C for 1 hour. It was then slowly warmed to room temperature and stirred for 15 hours, After which time it was cooled to 4 0C and quenched with sequential addition of water (1.2 ml_), 10% aqueous solution of sodium hydroxide (1.2 ml_) and finally water (3.6 ml_). Diethyl ether (50 ml_) was then added and the solution was allowed to stir for 90 minutes. The organic layer was separated and the aqueous phase was back extracted with diethyl ether (3 x 50 ml_). The combined organic layers were dried over magnesium sulphate, filtered, and concentrated under reduced pressure to give a 45% solution of the title compound in diethyl ether (1.56 g, 92%). 1H-NMR (400 MHz, CDCI3): delta 2.30 (m, 3H), 2.60 (m, 2H), 3.65 (m, 2H).
The synthetic route of 681128-38-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; PFIZER LIMITED; GIBSON, Karl Richard; GREEN, Martin Peter; UNDERWOOD, Toby James; WAKENHUT, Florian; WO2010/32200; (2010); A1;,
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