Electric Literature of 123-06-8, These common heterocyclic compound, 123-06-8, name is Ethoxymethylenemalononitrile, 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 mixture of Et3N (1.39 mL, 10 mmol) and cyclohexylhydrazine hydrochloride (1.51 g, 10 mmol) in EtOH (35 mL) was added ethoxymethylenemalononitrile (1.22 g, 10 mmol) portion wise. The reaction mixture was heated at reflux for 5 h, then cooled to room temperature and concentrated in vacuo. The residue was taken up in EtOAc (50 mL) and washed with water (2 x 25 mL). The organic phase was dried over Mg504, filtered and concentrated in vacuo to return 5-amino-1-cyclohexyl-pyrazole-4-carbonitrile (1.95 g, 103%) as an orange solid which was used without further purification. 1H NMR (300 MHz, CDCI3) O 7.49 (5, 1H), 4.45 (5, 2H), 3.77 (tt, =J= 11.2, 4.2 Hz, 1H), 1.88 (ddt, =J= 17.4, 11.4, 5.4 Hz, 6H), 1.83-1.65 (m, 1H), 1.49-1.32 (m, 1H), 1.38-1.15 (m, 2H).
The synthetic route of 123-06-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; CANCER RESEARCH TECHNOLOGY LIMITED; JORDAN, Allan; NEWTON, Rebecca; (145 pag.)WO2017/178845; (2017); A1;,
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