2-((4-METHOXYPHENYLAMINO)METHYLENE)MALONIC ACID DIETHYL ESTER synthesis
- Product Name:2-((4-METHOXYPHENYLAMINO)METHYLENE)MALONIC ACID DIETHYL ESTER
- CAS Number:83507-70-4
- Molecular formula:C15H19NO5
- Molecular Weight:293.32
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
226881-95-4
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