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ChemicalBook CAS DataBase List 2-((4-METHOXYPHENYLAMINO)METHYLENE)MALONIC ACID DIETHYL ESTER

2-((4-METHOXYPHENYLAMINO)METHYLENE)MALONIC ACID DIETHYL ESTER synthesis

5synthesis methods
-

Yield:83507-70-4 100%

Reaction Conditions:

at 14 - 95; for 2.91667 h;

Steps:

1

3.5 kg of p-anisidine are added to 6.25 kg of diethyl ethoxymethylenemalonate at 14° C., over 85 minutes without cooling of the reaction mass. At the end of addition, the temperature has reached 59° C. The temperature is kept at 59° C. for 30 minutes, and the reaction medium is then heated to 90-95° C. and kept at this temperature for 1 hour. The ethanol formed is then removed by distillation at atmospheric pressure and then under 250 mbar. After cooling to 45° C., 8.4 kg of diethyl 2-[(4-methoxyphenylamino)methylene]malonate are recovered in the form of a brown viscous oil, with a quantitative yield. Titer (HPLC.): 98.3%

References:

US2005/182259,2005,A1 Location in patent:Page/Page column 5