Electric Literature of 52133-67-2, A common heterocyclic compound, 52133-67-2, name is Ethyl 2-cyano-4,4-diethoxybutyrate, molecular formula is C11H19NO4, 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.
To a solution of sodium ethoxide (210 mL, 563 mmol; 21 percent in EtOH) in absolute EtOH (290 mL) were added ethyl-2-cyano-4,4-diethoxybutanoate (45 g, 281 mmol) and 2,2- dimethyl-propionamidine (59 g, 256 mmol) and heated to reflux for 12 h. The mixture was concentrated, the residue was diluted with water (100 mL) and acidified (pH 6-7) with aqueous 2N HC1 solution. The precipitate was filtered, dried under vacuum and dissolved in EtOH (100 mL). H2S04 (10 mL) was added at 0 ¡ãC and the mixture was heated to reflux for 2 h. After cooling to 25 ¡ãC the solution was made basic (pH~8-9) with NH3 aq.. The precipitate was filtered and dried under vacuum to yield 2-tert-butyl-l, 7-dihydro-pyrrolo [2,3-d]pyrimidin-4-one (18 g, 47percent) as white solid which was used in the next step without further purification. MS(m/e): 192 (M+H).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; GRETHER, Uwe; KIMBARA, Atsushi; NETTEKOVEN, Matthias; ROEVER, Stephan; ROGERS-EVANS, Mark; SCHULZ-GASCH, Tanja; WO2014/177527; (2014); A1;,
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