Reacción #2358564

Ecuación de reacción

ivabradine

acetonitrile hydrochloric acid

→

ivabradine hydrochloride

Rendimiento 75.0%

Disolventes

acetonitrile

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturamaintained for 60 minutes
2. 2
   FiltraciónThe product was filtered under nitrogen
3. 3
   Lavadowashed with chilled acetonitrile
4. 4
   workup.STIRRINGstirred for 30 min
5. 5
   TemperaturaThe reaction mixture was gradually cooled to 25° C.
6. 6
   workup.STIRRINGstirred for 1 hour
7. 7
   FiltraciónThe product was filtered under vacuum and nitrogen atmosphere
8. 8
   LavadoThe wet-cake was washed with chilled acetonitrile
9. 9
   OtroThe product was dried under vacuum at 50-55° C.

Procedimiento

100 g of ivabradine base and 300 mL acetonitrile were cooled to 0° C. to 5° C. and acetonitrile hydrochloric acid solution was added drop wise by adjusting the pH to about 1-2. The resulting mass was stirred till complete precipitation and maintained for 60 minutes. The product was filtered under nitrogen and washed with chilled acetonitrile. The wet-cake and acetonitrile were heated at 60-65° C. and stirred for 30 min. The reaction mixture was gradually cooled to 25° C. and stirred for 1 hour. The product was filtered under vacuum and nitrogen atmosphere. The wet-cake was washed with chilled acetonitrile. The product was dried under vacuum at 50-55° C. to obtain 75% 80 g crude ivabradine hydrochloride. The product was packed in double polyethene bag under nitrogen.

Fuente