Toluene → Clopidogrel Besylate

HRID 15387

반응식

HRID 15387 반응식
[CH3:1][O:2][C:3]([C@@H:5]([N:13]1[CH2:21][C:17]2[CH:18]=[CH:19][S:20][C:16]=2[CH2:15][CH2:14]1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=1[Cl:12])=[O:4].[C:22]1([S:28]([OH:31])(=[O:30])=[O:29])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C1(C)C=CC=CC=1>CO>[CH3:1][O:2][C:3]([C@@H:5]([N:13]1[CH2:21][C:17]2[CH:18]=[CH:19][S:20][C:16]=2[CH2:15][CH2:14]1)[C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:4].[CH:25]1[CH:26]=[CH:27][C:22]([S:28]([OH:31])(=[O:30])=[O:29])=[CH:23][CH:24]=1

참가 물질

5

반응물 3

HCID 1140TolueneHCID 7371Benzenesulfonic AcidHCID 60606Clopidogrel

생성물 1

HCID 9847991Clopidogrel Besylate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Clopidogrel base was dissolved in methanol. Benzene sulphonic acid was added to the solution at 20° C. The reaction mixture was heated to reflux temperature for 2 hrs. The solution was cooled to room temperature and the methanolic solution was added drop-wise to the boiling toluene. The resulting solution was refluxed for an additional 20 minutes. The solution was cooled to room temperature and was stirred at this temperature for extended hours. The solvent was evaporated under reduced pressure to dryness to obtain Clopidogrel besylate, similar to that obtained above.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux temperature for 2 hrs
  3. temperatureThe resulting solution was refluxed for an additional 20 minutes
  4. temperatureThe solution was cooled to room temperature
  5. customThe solvent was evaporated under reduced pressure to dryness

출처 및 근거

ORD 기록
ord-79e42ee156964036b3247b842e37d4c7
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732608B2

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