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Morpholine → Morpholine, 4-(2-chloro-4-nitrophenyl)-

HRID 56227
ノート
印刷プレビュー

反応式

HRID 56227 の反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[Cl:7][C:8]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[CH:11]=[CH:10][C:9]=1F.CCN(CC)CC>CN(C=O)C>[Cl:7][C:8]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[CH:11]=[CH:10][C:9]=1[N:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8083MorpholineHCID 8471TriethylamineHCID 676882-Chloro-1-fluoro-4-nitrobenzene

生成物 1

HCID 108711Morpholine, 4-(2-chloro-4-nitrophenyl)-収率 63.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of morpholine (1.1 mL, 12.6 mmol) in DMF (30 mL) were added 2-chloro-1-fluoro-4-nitrobenzene (1.76 g, 10.0 mmol) and Et3N (4.2 mL, 30.1 mmol) with stirring and the mixture was stirred at rt overnight. The mixture was then filtered and the organic phase was poured into 150 mL of DCM, washed with water (150 mL×3) and brine (150 mL), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/DCM (V/V)=10:1) to give the title compound as a yellow solid (1.53 g, 63%).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. stirringthe mixture was stirred at rt overnight
  2. filtrationThe mixture was then filtered
  3. additionthe organic phase was poured into 150 mL of DCM
  4. washwashed with water (150 mL×3) and brine (150 mL)
  5. dry with materialdried over anhydrous Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by a silica gel column chromatography (PE/DCM (V/V)=10:1)

出典と根拠

ORDレコード
ord-f4072d50c2dc4c7bb60dd7a9c543384b
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434695B2

反応ノート

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