Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 40497-11-8, name is Ethyl 2,3-dicyanopropanoate, A new synthetic method of this compound is introduced below., Recommanded Product: Ethyl 2,3-dicyanopropanoate
Example 11Preparation of 5-aminopyrazole (VII):; To 2,6-dichloro-4-trifluoromethyl aniline 230 g and acetic acid 150 ml was added 1.1m of nitrosyl sulphuric acid over one hour at 30C and maintained at 30C for one more hour. Heat the mass to 50-55C over ? hour and the absence of 2,6-dichloro-4-trifluoromethyl aniline was monitored. Cool the mass to 30C, and the excess nitrosyl sulphuric acid was destroyed.The above diazotized mass was added to a mixture of 250 ml of acetic acid, 162 g ethyl-2,3-dicyanoproprionate and 425 ml water over 4-5 hours maintaining temperature 0-5C. Further maintained at 0C / 2 hours, 5C / 1 hour, 10C / lhour, 15C / 1 hour. 800 ml water was added at 15C over ? hour, extracted the solution with 3×250 ml methylene dichloride. Layers were separated. Dichloromethane layer was washed with 250 ml water, cooled the dichloromethane layer to 0C and washed with 250 ml 8N aq. NH3 under stirring for one hour. Layers were separated, dichloromethane layer was taken and NH3 gas was passed at 0-5 C till free NH3 was observed on top of the condenser and maintained the reaction mass for 3-4 hours at 0-5C. Then 250 ml water was added, stirred for ? hour, layers were separated, extracted aq. layer with 2×100 ml dichloromethane, dichloromethane layer was dried with MgS04, dichloromethane layer was concentrated to dryness, to obtain 288 g of 5-amino-3-cyano-l-(2,6- dichloro-4-triflouromethyl phenyl)-pyrazole of 98% purity.
The synthetic route of 40497-11-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GHARDA, Keki Hormusji; WO2011/107998; (2011); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts