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Hydrochloric Acid → 1-[5-[(Z)-2-cyano-2-(3,4-dimethoxy-phenyl)-vinyl]-thiophen-2-yl]-piperidin-4-yl diethylamino-acetate hydrochloride

HRID 2366446
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HRID 2366446 반응식
[ClH:1].[CH2:2]([N:4]([CH2:7][C:8]([O:10][CH:11]1[CH2:16][CH2:15][N:14]([C:17]2[S:18][C:19](/[CH:22]=[C:23](\[C:34]#[N:35])/[C:24]3[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[C:26]([O:32][CH3:33])[CH:25]=3)=[CH:20][CH:21]=2)[CH2:13][CH2:12]1)=[O:9])[CH2:5][CH3:6])[CH3:3]>C(O)(C)C>[ClH:1].[CH2:2]([N:4]([CH2:7][C:8]([O:10][CH:11]1[CH2:12][CH2:13][N:14]([C:17]2[S:18][C:19](/[CH:22]=[C:23](\[C:34]#[N:35])/[C:24]3[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[C:26]([O:32][CH3:33])[CH:25]=3)=[CH:20][CH:21]=2)[CH2:15][CH2:16]1)=[O:9])[CH2:5][CH3:6])[CH3:3]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 11964785YHO-13351 free base

생성물 1

HCID 672278271-[5-[(Z)-2-cyano-2-(3,4-dimethoxy-phenyl)-vinyl]-thiophen-2-yl]-piperidin-4-yl diethylamino-acetate hydrochloride수율 70%

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
80 °C

실험 절차

Isopropanol (10 mL) and 12N hydrochloric acid (59 μL) were added to Compound 103 (338 mg), and the mixture was heated for dissolution (external temperature: 80° C.). The solution was returned to room temperature, and allowed to stand overnight. The precipitated crystals were recovered through filtration, and the recovered crystals were recrystallized from isopropanol, to thereby yield the target product (yield: 254.5 mg, 70.0%).

후처리

  1. customwas returned to room temperature
  2. filtrationThe precipitated crystals were recovered through filtration
  3. customthe recovered crystals were recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-beaf8c2abfb24d4490b8c8b91318414a
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697742B2

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