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Ethyl 3-(2-nitrobenzyl)-2-oxo-1-propyl-3-piperidinecarboxylate → HCID 18332960、化合物

HRID 2269722
ノート
印刷プレビュー

反応式

HRID 2269722 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

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

生成物 1

HCID 18332960HCID 18332960、化合物収率 70.4%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-588de430343d40ec81df83959d8b1201
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06329389B1

反応ノート

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