反应详情

温度

25 °C

Potassium cyanide (6.1 Kg) was dissolved in methanol (119 Kg) at 50° C. over 1 hour. Aminoacetamidine dihydrobromide (19.6 Kg) was added to the potassium cyanide solution in one portion and stirred at 25° C. for 15 minutes to allow formation of the mono acid mono hydrocyanide salt. Subsequently, 2,3,5-trichlorobenzaldehyde (24.2 Kg) was added to the reaction mixture in one portion and the mixture was stirred at 50° C. for 16 hours. On cooling to 25° C., vacuum was applied and the mixture concentrated to 5 volumes. Isopropyl ether (145 Kg) was added over 30 minutes and the mixture stirred at 20° C. overnight. The crude product was isolated by filtration and the cake washed with isopropyl ether (43 Kg). The crude product was slurried with ethyl acetate (158 kg). and water (100 kg) overnight at 20° C. The product was isolated by filtration washed with water (50 Kg), ethyl acetate (90 Kg) and vacuum dried at 400C to afford 2-{[Cyano-(2,3,5-trichlorophenyl)-methyl]-amino}-acetamidine hydrobromide. Yield 17.43 Kg (50% -92% w/w assay). HPLC retention time 3.9 minutes.

1. stirringthe mixture was stirred at 50° C. for 16 hours
2. temperatureOn cooling to 25° C.
3. concentrationthe mixture concentrated to 5 volumes
4. additionIsopropyl ether (145 Kg) was added over 30 minutes
5. stirringthe mixture stirred at 20° C. overnight
6. customThe crude product was isolated by filtration
7. washthe cake washed with isopropyl ether (43 Kg)
8. customwater (100 kg) overnight
9. customat 20° C
10. customThe product was isolated by filtration
11. washwashed with water (50 Kg), ethyl acetate (90 Kg) and vacuum
12. dry with materialdried at 400C