Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 52133-67-2, name is Ethyl 2-cyano-4,4-diethoxybutyrate, This compound has unique chemical properties. The synthetic route is as follows., 52133-67-2
To a microwave reaction tube was charged with 37 (1.1 g, 5.0 mmol), 2-cyano-4,4- diethoxy-butyric acid ethyl ester (1.7 g, 7.4 mmol) and NaOMe (25percent by wt in MeOH; 10 mL). The reaction tube was sealed and the solution irradiated with microwave at 150 0C for 30 min. After cooling to room temperature, the mixture was concentrated. The residue was taken up in water (10 mL) and the pH adjusted to 1 with 6M of HCl. The resulting solution was stirred at room temperature for 25 min and then the pH adjusted to 9 with concentrated NH4OH. The resulting solid was filtered, washed with water and dried under high vacuum to afford the title compound as a grey solid (1.5 g, 94percent). The material was used in the next step without purification.[0234] 1H NMR (500 MHz, DMSO-J6) delta 2.25 (s, 3H), 5.07 (s, 2H), 6.29 (dd, J = 3.0, 2.2 Hz, IH), 6.75 (t, J = 2.7 Hz, IH), 6.76 (d, J = 0.7 Hz, IH), 7.09-7.15 (m, 3H), 7.60 (d, J = 8.5 Hz, 2H), 8.71 (s, IH), 10.28 (br s, IH), 11.36 (s, IH) MS (ES+): m/z 321 (M+H)+
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Reference:
Patent; TARGEGEN INC.; WO2009/49028; (2009); A1;,
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