反应详情

温度

-10 °C

Lithium hydroxide monohydrate (2.9 kg) was stirred in methanol (269 kg) for 60 minutes at 20° C. and then cooled to −10C. 2-{[Cyano-(2,3,5-trichlorophenyl)-methyl]-amino}-acetamidine hydrobromide was added in one portion and the resultant mixture stirred vigorously with cooling at −10° C. Compressed air was gassed over the surface of the reaction for at least 6 hours. The mixture was warmed to 25° C. and concentrated to 3 volumes under vacuum. Water (289 kg) was added over at least 1 hour with stirring. The product was isolated by filtration and the cake washed with water (51 kg) and dried in vacuo at 40° C. Yield 12 Kg (91%). HPLC retention time 11.9 minutes.

1. temperaturecooled to −10C
2. customCompressed air was gassed over the surface of the reaction for at least 6 hours
3. temperatureThe mixture was warmed to 25° C.
4. concentrationconcentrated to 3 volumes under vacuum
5. additionWater (289 kg) was added over at least 1 hour
6. customThe product was isolated by filtration
7. washthe cake washed with water (51 kg)
8. customdried in vacuo at 40° C