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Ethanol → HCID 18332987、化合物

HRID 2269720
ノート
印刷プレビュー

反応式

HRID 2269720 の反応式
[H-].[Na+].C(O)C.[C:6]([CH:11]1[CH2:16][CH2:15][CH2:14][NH:13][C:12]1=[O:17])([O:8][CH2:9][CH3:10])=[O:7].[N+:18]([C:21]1[CH:28]=[CH:27][CH:26]=[CH:25][C:22]=1[CH2:23]Br)([O-:20])=[O:19]>O>[N+:18]([C:21]1[CH:28]=[CH:27][CH:26]=[CH:25][C:22]=1[CH2:23][C:11]1([C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:16][CH2:15][CH2:14][NH:13][C:12]1=[O:17])([O-:20])=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 702EthanolHCID 24758Sodium hydrideHCID 77569alpha-Bromo-2-nitrotolueneHCID 977733-Carbethoxy-2-piperidone

生成物 1

HCID 18332987HCID 18332987、化合物収率 81.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Sodium hydride (60% dispersion in oil, 2.45 g) was added to ethanol (100 ml), to which was added 3-carboethoxy-2-piperidone (10.0 g). The reaction mixture was stirred for 15 minutes, to which was added 2-nitrobenzyl bromide (13.2 g) at room temperature. The reaction mixture was stirred at 60° C. for 3 hours. Water was added to the reaction mixture, which was concentrated. The residue was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, then dried and concentrated. The obtained crude crystals were recrystallized from ethyl acetate-hexane to give the entitled compound (14.6 g).

後処理

  1. stirringThe reaction mixture was stirred at 60° C. for 3 hours
  2. concentrationwas concentrated
  3. additionThe residue was diluted with water
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with water
  6. dry with materiala saturated aqueous sodium chloride solution, then dried
  7. concentrationconcentrated
  8. customThe obtained crude crystals
  9. customwere recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-5d6b7880a5f6456c8ce13d06b61535fd
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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