반응 #2358564

반응 방정식

ivabradine

acetonitrile hydrochloric acid

→

ivabradine hydrochloride

수율 75.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도maintained for 60 minutes
2. 2
   여과The product was filtered under nitrogen
3. 3
   세척washed with chilled acetonitrile
4. 4
   workup.STIRRINGstirred for 30 min
5. 5
   온도The reaction mixture was gradually cooled to 25° C.
6. 6
   workup.STIRRINGstirred for 1 hour
7. 7
   여과The product was filtered under vacuum and nitrogen atmosphere
8. 8
   세척The wet-cake was washed with chilled acetonitrile
9. 9
   기타The product was dried under vacuum at 50-55° C.

실험 절차

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.

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