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Ethyl 3-(2-nitrobenzyl)-2-oxo-1-propyl-3-piperidinecarboxylate → HCID 18332960, 화합물

HRID 2269722
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HRID 2269722 반응식
[N+:1]([C:4]1[CH:25]=[CH:24][CH:23]=[CH:22][C:5]=1[CH2:6][C:7]1([C:17](OCC)=[O:18])[CH2:12][CH2:11][CH2:10][N:9]([CH2:13][CH2:14][CH3:15])[C:8]1=[O:16])([O-])=O>[C].[Pd].C(O)C>[O:16]=[C:8]1[C:7]2([CH2:6][C:5]3[C:4](=[CH:25][CH:24]=[CH:23][CH:22]=3)[NH:1][C:17]2=[O:18])[CH2:12][CH2:11][CH2:10][N:9]1[CH2:13][CH2:14][CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 18332952Ethyl 3-(2-nitrobenzyl)-2-oxo-1-propyl-3-piperidinecarboxylate

생성물 1

HCID 18332960HCID 18332960, 화합물수율 70.4%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매

실험 절차

10% Palladium- carbon (0.2 g) was added to an ethanol solution (20 ml) of ethyl 3-(2-nitrobenzyl)-2-oxo-1-propyl-3-piperidinecarboxylate (1.00 g), and catalytic hydrogenation was conducted at room temperature under one atmospheric pressure for 6 hours. The catalyst was removed by filtration and the filtrate was concentrated. The residue was dissolved in toluene (20 ml), which was heated under reflux for 12 hours. The reaction mixture was concentrated, and the obtained crude crystals were recrystallized from ethyl acetate-hexane to give the entitled compound (0.55 g).

후처리

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated
  3. dissolutionThe residue was dissolved in toluene (20 ml)
  4. temperaturewhich was heated
  5. temperatureunder reflux for 12 hours
  6. concentrationThe reaction mixture was concentrated
  7. customthe obtained crude crystals
  8. customwere recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-588de430343d40ec81df83959d8b1201
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06329389B1

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