Application of 52133-67-2,Some common heterocyclic compound, 52133-67-2, name is Ethyl 2-cyano-4,4-diethoxybutyrate, molecular formula is C11H19NO4, 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.
The compound (1) (30.0 g, 0.313 mol) was added to a suspension of sodium hydride (3.77 g, 0.617 mol) in dimethylformamide (100 ml) under nitrogen atmosphere below 20° C., and the mixture was stirred at room temperature for 30 min. To the resulting mixture was added 2-(3-chloropropyl)tetrahydro-2H-pyran (25.7 g, 0.144 mol) at the same temperature, then the mixture was stirred in an oil bath at 60° C. for 16 h. The reaction mixture is evaporated under reduced pressure to remove dimethylformamide, to the residue was added water and the mixture was extracted with toluene. After the toluene layer was washed with water, dried over magnesium sulfate, and evaporated to remove toluene, the excess of 2-(3-chloropropyl)tetrahydro-2H-pyran was distilled and removed in an oil bath at 150° C. under reduced pressure to give the compound (2) (41.5 g, 85.4percent). [00174] 1H NMR (CDCl3); 1.18 (3H, t, J=6.9 Hz), 1.21 (3H, t, J=6.9 Hz), 1.33 (3H, t, J=7.2 Hz), 1.52-2.04 (12H, m), 2.40 (1H, m), 3.39-3.86 (7H, m), 4.24 (2H, m), 4.57 (1H, m), 4.77 (1H, m).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 2-cyano-4,4-diethoxybutyrate, its application will become more common.
Reference:
Patent; Shionogi & Co., Ltd.; US6756376; (2004); B1;,
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