反应详情

There are introduced into a 670 litre reactor 85.0 kg of 7-methoxy-1-tetralone, 60.3 kg of cyanoacetic acid and 15.6 kg of heptanoic acid in toluene in the presence of 12.7 kg of benzylamine. The mixture is heated at reflux. When all the starting substrate has disappeared, the solution is cooled and filtered. The precipitate obtained is washed with toluene and then the filtrate obtained is washed with a 2N sodium hydroxide solution and subsequently with water until neutral. After removal of the solvent by evaporation, the resulting solid is recrystallised from an ethanol/water (80/20) mixture to give the title product in a yield of 90% and with a chemical purity exceeding 99%.

1. temperatureThe mixture is heated
2. temperatureat reflux
3. temperaturethe solution is cooled
4. filtrationfiltered
5. customThe precipitate obtained
6. washis washed with toluene
7. customthe filtrate obtained
8. washis washed with a 2N sodium hydroxide solution and subsequently with water until neutral
9. customAfter removal of the solvent
10. customby evaporation
11. customthe resulting solid is recrystallised from an ethanol/water (80/20) mixture