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Hydrochloric Acid → Prasugrel Hydrochloride

HRID 1428167
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HRID 1428167 반응식
[CH3:1][C:2]([O:4][C:5]1[S:9][C:8]2[CH2:10][CH2:11][N:12]([CH:14]([C:22]([CH:24]3[CH2:26][CH2:25]3)=[O:23])[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:20]=3[F:21])[CH2:13][C:7]=2[CH:6]=1)=[O:3].[ClH:27]>CC(C)=O>[CH3:1][C:2]([O:4][C:5]1[S:9][C:8]2[CH2:10][CH2:11][N:12]([CH:14]([C:22]([CH:24]3[CH2:26][CH2:25]3)=[O:23])[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:20]=3[F:21])[CH2:13][C:7]=2[CH:6]=1)=[O:3].[ClH:27]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 6918456Prasugrel

생성물 1

HCID 10158453Prasugrel Hydrochloride수율 90%

시약·촉매·용매 1

HCID 180Acetone용매2회

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온도
20 °C

실험 절차

Prasugrel free base prepared by example 3 (2.0 g) disclosed herein was dissolved in acetone (25 ml) with stirring at 20° C. until complete dissolution and the mixture was further stirred for 10 minutes. A solution of hydrochloric acid in acetone (0.46 ml hydrochloric acid (37 wt. %) dissolved in 5 ml acetone) was added slowly to the reaction mixture over 1 hour at 20° C. After the addition, a seed crystal (0.05 g) (crystalline form B2 of prasugrel hydrochloride), the resulting mixture was stirred at 20° C. for 15 hours followed by filtration. The obtained crystal was washed with acetone and dried under vacuum at 50° C. for 24 hours. The resulting product was prasugrel hydrochloride crystalline Form B2 with the HPLC purity of 99.74%. The yield was 90%.

후처리

  1. stirringthe mixture was further stirred for 10 minutes
  2. additionAfter the addition
  3. filtrationfollowed by filtration
  4. washThe obtained crystal was washed with acetone
  5. customdried under vacuum at 50° C. for 24 hours

출처 및 근거

ORD 기록
ord-8ea2865ae1c7402bbd5be984e4be41ce
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08937053B2

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