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Triethylamine → HCID 70665405、化合物

HRID 333542
ノート
印刷プレビュー

反応式

HRID 333542 の反応式
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[CH:11]1[C:19]2[C:18]3[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=3[O:16][C:15]=2[C:14]([NH2:24])=[CH:13][CH:12]=1.C(N(CC)CC)C>C(O)CCC>[CH:11]1[C:19]2[C:18]3[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=3[O:16][C:15]=2[C:14]([NH:24][C:2]2[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=2)=[CH:13][CH:12]=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 8471TriethylamineHCID 796132-Chloro-3-nitropyridineHCID 4593514-Dibenzofuranamine

生成物 1

HCID 70665405HCID 70665405、化合物

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

2-chloro-3-nitropyridine (4.39 g, 27.7 mmol), dibenzo[b,d]furan-4-amine (5.58 g, 30.5 mmol), triethylamine (4.3 mL, 30.9 mmol), and butanol (90 mL) were mixed in a 250 mL round bottom flask. The reaction mixture was refluxed overnight under nitrogen. The solvent was evaporated, leaving an orange solid which was dried under vacuum. The solid was taken up in ethyl acetate, water was added and the layers were separated. The organic layer with washed with brine, dried over magnesium sulfate, filtered, and evaporated to a residue. The residue was purified on by column chromatography eluting with 10% ethyl acetate/hexanes followed by ethyl acetate (4.6 g, 54%).

後処理

  1. temperatureThe reaction mixture was refluxed overnight under nitrogen
  2. customThe solvent was evaporated
  3. customleaving an orange solid which
  4. customwas dried under vacuum
  5. additionwater was added
  6. customthe layers were separated
  7. washThe organic layer with washed with brine
  8. dry with materialdried over magnesium sulfate
  9. filtrationfiltered
  10. customevaporated to a residue
  11. customThe residue was purified on by column chromatography
  12. washeluting with 10% ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-78478ba2e325449491610abf7ec88fa0
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883322B2

反応ノート

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