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63010-68-4

2-[(2-Fluoro-phenylaMino)-Methylene]-Malonic acid diethyl ester synthesis

3synthesis methods
-

Yield:63010-68-4 93.4%

Reaction Conditions:

at 100; for 3 h;Inert atmosphere;

Steps:



A mixture of compounds 1 (17.78 g, 0.16 mol) and 2 (37.36 g, 0.l7mol) washeated at 100 °C under atmosphere of nitrogen for 3 hours. The resulting solutionwas cooled down followed by dilution with hexane (100 mL). The mixture was then stirred at 60 °C for one hour and allowed to cool down to room temperature. The precipitated solid was filtered, washed with hexane (3 x 50 mL) and dried to yield compound 3 (42 g, 93.4 %) as a white solid, which was used directly in the next stepwithout further purification. LRMS (M+H) m/z: calcd. 282.12; found 282.12.

References:

WO2014/66506,2014,A2 Location in patent:Page/Page column 95