反応 #2358564

反応方程式

ivabradine

acetonitrile hydrochloric acid

→

ivabradine hydrochloride

収率 75.0%

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度maintained for 60 minutes
2. 2
   ろ過The product was filtered under nitrogen
3. 3
   洗浄washed with chilled acetonitrile
4. 4
   workup.STIRRINGstirred for 30 min
5. 5
   温度The reaction mixture was gradually cooled to 25° C.
6. 6
   workup.STIRRINGstirred for 1 hour
7. 7
   ろ過The product was filtered under vacuum and nitrogen atmosphere
8. 8
   洗浄The wet-cake was washed with chilled acetonitrile
9. 9
   その他The product was dried under vacuum at 50-55° C.

実験手順

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.

出典