反应详情

With ice cooling and stirring, 40 ml of ethanol solution containing 3.6 g of ethyl 2-ethoxycarbonyl-2-[4-(2-ethoxy-2-iminoethoxy]phenyl]acetate obtained in the above step b) was added dropwise to a 10 ml ethanol solution containing 0.6 g of ethylenediamine, and the resulting mixture was stirred at room temperature for 1.5 hours, followed by refluxing under heating for 0.5 hours. After cooling, the resulting reaction solution was adjusted to an acidic pH with ethanol containing 13% (w/v) of hydrochloric acid, and then concentrated to dryness. The residue thus obtained was dissolved in water and washed with diethyl ether. Thereafter, the resulting water layer was adjusted to pH 9-10 with dilute sodium hydroxide aqueous solution, and crystals thus precipitated were collected by filtration. In this way, 1.83 g of the title compound was obtained in the form of colorless crystals.

1. customobtained in the above step b)
2. stirringthe resulting mixture was stirred at room temperature for 1.5 hours
3. temperatureby refluxing
4. temperatureunder heating for 0.5 hours
5. temperatureAfter cooling
6. customthe resulting reaction solution
7. concentrationconcentrated to dryness
8. customThe residue thus obtained
9. washwashed with diethyl ether
10. customthus precipitated
11. filtrationwere collected by filtration