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Hydrogen chloride-ethyl acetate → 3-[2-(4-Piperidinyl)ethyl]benzamide hydrochloride

HRID 2074243
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반응식

HRID 2074243 반응식
[NH2:1][C:2]([C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][CH:12]2[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14][CH2:13]2)[CH:7]=[CH:8][CH:9]=1)=[O:3].[ClH:25].CCOC(C)=O>CCOC(C)=O>[ClH:25].[NH:15]1[CH2:16][CH2:17][CH:12]([CH2:11][CH2:10][C:6]2[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=2)[C:2]([NH2:1])=[O:3])[CH2:13][CH2:14]1
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참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 57421827Tert-butyl 4-{2-[3-(aminocarbonyl)phenyl]ethyl}-1-piperidinecarboxylate

생성물 1

HCID 574218283-[2-(4-Piperidinyl)ethyl]benzamide hydrochloride

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Tert-butyl 4-{2-[3-(aminocarbonyl)phenyl]ethyl}-1-piperidinecarboxylate (13.8 g) was dissolved in EtOAc (200 ml), and 4 M hydrogen chloride/EtOAc solution (130 ml) was added thereto, followed by stirring at room temperature for 4 hours, and then concentrated. Acetonitrile was added to the resulting residue, followed by heating, and the precipitated crystal was collected by filtration, washed with EtOAc, and dried under reduced pressure to obtain 3-[2-(4-piperidinyl)ethyl]benzamide hydrochloride (11.2 g).

후처리

  1. concentrationconcentrated
  2. additionAcetonitrile was added to the resulting residue
  3. temperatureby heating
  4. filtrationthe precipitated crystal was collected by filtration
  5. washwashed with EtOAc
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-10cee70ee7c74a9aa9fbaef612b46210
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07919494B2

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