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Carbon Dioxide → 2-(4-aminophenyl)-N-methylacetamide

HRID 1080695
ノート
印刷プレビュー

反応式

HRID 1080695 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][C:11]([OH:13])=O)=[CH:6][CH:5]=1)([O-])=O.[C:14](N1C=CN=C1)([N:16]1C=CN=C1)=O.C(=O)=O>C1COCC1>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][C:11]([NH:16][CH3:14])=[O:13])=[CH:6][CH:5]=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 280Carbon DioxideHCID 4661(4-Nitrophenyl)acetic acidHCID 682631,1'-Carbonyldiimidazole

生成物 1

HCID 167753762-(4-aminophenyl)-N-methylacetamide収率 66.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4-Nitrobenzeneacetic acid (16.6 g, 0.0916 mol) was dissolved in THF (200 mL) and carbonyldiimidazole (CDI, 15.6 g, 0.0963 mol) was added. Carbon dioxide evolution rapidly ensued and the reaction mixture was stirred at RT for 30 min. Gaseous methylamine was then bubbled through the mixture until it was distinctly basic to litmus paper. The THF was removed in vacuo and water (70 mL) was added. The solid material was collected by filtration and placed in a Parr bottle were palladium on carbon (10%, 3 g). A solution of EtOH (200 mL) and 1N HCl (50 mL) was added and the mixture was hydrogenated at 60 psi for 4 h. The reaction was filtered, concentrated in vacuo and the residue made basic with saturated aqueous Na2CO3. The aqueous mixture was extracted with EtOAc. The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated in vacuo to give the product (6) (10.0 g, 66.6%) which was pure by NMR analysis.

後処理

  1. customGaseous methylamine was then bubbled through the mixture until it
  2. customThe THF was removed in vacuo and water (70 mL)
  3. additionwas added
  4. filtrationThe solid material was collected by filtration
  5. additionA solution of EtOH (200 mL) and 1N HCl (50 mL) was added
  6. waitthe mixture was hydrogenated at 60 psi for 4 h
  7. filtrationThe reaction was filtered
  8. concentrationconcentrated in vacuo
  9. extractionThe aqueous mixture was extracted with EtOAc
  10. washThe combined organic layers were washed with brine
  11. dry with materialdried over MgSO4
  12. filtrationfiltered
  13. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-56e3cf8b2f7a4bf3901240936f46faa1
出典データセット
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05583149

反応ノート

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