As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 123-06-8 name is Ethoxymethylenemalononitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 123-06-8
To a mixture of commercially available cyclopentylhydrazine hydrochloride(R-i4b) (1.82 g, 18.18 mmol) and commercially available compound 4:(ethoxymethylene)malononitrile (1.34 g, 10.97 mmol) in EtOH (20 mL), was added Et3N (3.03 g, 29.93 mmol) in one portion at r.t. under N2. The mixture was stirred at r.t. for 10 mm. Then heated to 50C and stirred for 2 hrs. The mixture was cooled to r.t. and concentrated in reduced pressure. The residuewas poured into water and the aqueous phase was extracted with EA (50 mL). The combined organic phase was washed with saturated brine (20 mL), dried with anhydrous Na2SO4, filtered and concentrated in vacuum. The residue was purified by silica gel chromatography to afford intermediate I-44b (1 .22 g, 69% yield) as yellow solid. ESI-MS (Mi-i): 177.1 calc. for C9H12N4: 176.1.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethoxymethylenemalononitrile, and friends who are interested can also refer to it.
Reference:
Patent; FUNDACION PARA LA INVESTIGACION MEDICA APLICADA; CUADRADO TEJEDOR, Maria Del Mar; FRANCO FERNANDEZ, Rafael; GARCIA OSTA, Ana Maria; OYARZABAL SANTAMARINA, Julen; RABAL GRACIA, Maria Obdulia; WO2014/131855; (2014); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts