Some common heterocyclic compound, 6136-93-2, name is 2,2-Diethoxyacetonitrile, molecular formula is C6H11NO2, 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. Quality Control of 2,2-Diethoxyacetonitrile
Into a 100-mL round bottom flask was placed a solution of 2,2-diethoxyacetonitrile (5.00 g, 38.83 mmol) and sodium methylate(30% in methanol, 1 mL) in methanol (30 mL)at ambient temperature. The resulting mixture was degassed with nitrogen for3 times and stirred at room temperature for 42 hr. The reaction was quenched with solid CO2and evaporated under vacuum. The residue was diluted with water (100 mL) and extracted with dichloromethane (3 xlOO mL). The combined organics were washed with brine(200 mL),dried over anhydrous sodium sulfate and filtered. The solvent was evaporated under vacuum to yieldthe title compound:?H NMR (400 MHz, CD3C1): oe7.89 (s, 1H), 4.80 (s, 1H),3.81 (s, 3H), 3.60-3.52 (m, 4H), 1.29-1.22 (m, 6H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6136-93-2, its application will become more common.
Reference:
Patent; MERCK SHARP & DOHME CORP.; BENNETT, Frank; JIANG, Jinlong; PASTERNAK, Alexander; DONG, Shuzhi; GU, Xin; SCOTT, Jack D.; TANG, Haiqun; ZHAO, Zhiqiang; HUANG, Yuhua; HUNTER, David; YANG, Dexi; ZHANG, Zhibo; FU, Jianmin; BAI, Yunfeng; ZHENG, Zhixiang; ZHANG, Xu; YOUNG, Katherine; XIAO, Li; (580 pag.)WO2016/206101; (2016); A1;,
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