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ChemicalBook CAS DataBase List 3-CYANO-BETA-OXO-BENZENEPROPANOIC ACID METHYL ESTER
209731-74-8

3-CYANO-BETA-OXO-BENZENEPROPANOIC ACID METHYL ESTER synthesis

3synthesis methods
-

Yield:209731-74-8 86%

Reaction Conditions:

with sodium hydride in toluene at 100; for 2 h;Inert atmosphere;Reflux;

Steps:

C7 Example C7: Methyl 3- 3-cyanop eny -3-oxopropanoate:

Example C7: Methyl 3- 3-cyanop eny -3-oxopropanoate: [0151] Into a three-necked flask equipped with an argon inlet and a condenser were placed sodium hydride (60%>, 689.5 mg, 17.23 mmol), dimethyl carbonate (1.55 g, 17.23 mmol) and 15 mL of toluene. The mixture was stirred under reflux and a solution of 3- acetylbenzonitrile (1.0 g, 6.19 mmol) in toluene (15 mL) was added drop wise. The reaction mixture was stirred at 100°C for 2h. The reaction mixture was monitored by LCMS and purified by column chromatography on silica gel eluted with 0-10% of ethyl acetate in petroleum ether to give the product (1.2 g, 86%>).

References:

WO2013/33246,2013,A2 Location in patent:Paragraph 0151