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Acetone → (alphaS)-alpha-(2-Chlorophenyl)-6,7-dihydrothieno[3,2-c]pyridine-5(4H)-acetic acid hydrochloride (1:1)

HRID 2358440
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HRID 2358440 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C@H:8]([N:12]1[CH2:17][CH2:16][C:15]2[S:18][CH:19]=[CH:20][C:14]=2[CH2:13]1)[C:9]([OH:11])=[O:10].CC(C)=O.Cl>CO>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C@H:8]([N:12]1[CH2:17][CH2:16][C:15]2[S:18][CH:19]=[CH:20][C:14]=2[CH2:13]1)[C:9]([OH:11])=[O:10]
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참가 물질

5

반응물 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 9861403Clopidogrel carboxylic acid

생성물 1

HCID 45358950(alphaS)-alpha-(2-Chlorophenyl)-6,7-dihydrothieno[3,2-c]pyridine-5(4H)-acetic acid hydrochloride (1:1)수율 178.8%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
40 °C

실험 절차

61 g of (S)-(+)-α-(2-chlorophenyl)-6,7-dihydro-4H-thieno[3,2-c]pyridine-5-acetic acid obtained in Example 5 was added to a mixture of 300 ml of acetone and 15 ml of methanol, and then heated to 40° C. 16.4 ml of concentrated hydrochloric acid was added thereto, and the resulting mixture was stirred at room temperature for 2 hrs, and then, at below 5° C. for at least 2 hrs. The precipitated crystals were filtered, washed with 100 ml of acetone and dried at 40° C. under a reduced pressure, to obtain 61 g of the title compound as a white-yellow solid (yield: 90%).

후처리

  1. waitat below 5° C. for at least 2 hrs
  2. filtrationThe precipitated crystals were filtered
  3. washwashed with 100 ml of acetone
  4. customdried at 40° C. under a reduced pressure

출처 및 근거

ORD 기록
ord-b0deec71fef140dba1810b55e156d6b8
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07763730B2

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