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(2-Acetamidophenyl) cyclohexyl methanone → (2-Aminophenyl)(cyclohexyl)methanone

HRID 1490098
ノート
印刷プレビュー

反応式

HRID 1490098 の反応式
C([NH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]([CH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1)=[O:12])(=O)C>CO.Cl>[NH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]([CH:13]1[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18]1)=[O:12]
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 11586813(2-Acetamidophenyl) cyclohexyl methanone

生成物 1

HCID 15634733(2-Aminophenyl)(cyclohexyl)methanone収率 91.1%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

実験手順

A solution of (2-acetamidophenyl) cyclohexyl methanone (0.53 g) in methanol (5 ml) and concentrated hydrochloric acid (15 ml) was heated at 80° C. for 1 hour. After this time the solution was cooled to ambient temperature and the solvents removed in vacuo. The residue was dissolved in water (10 ml) and basified with 4N sodium hydroxide solution (20 ml). The mixture was then extracted into ethyl acetate (4×20 ml) and the organic layers combined and dried (MgSO4). The solvent was evaporated and the residue chromatographed on silica gel using petrol:ethyl acetate (2:1), to afford the title compound (0.40 g) as a solid. The spectroscopic properties of this material were identical to those described in Method A.

後処理

  1. customthe solvents removed in vacuo
  2. dissolutionThe residue was dissolved in water (10 ml)
  3. extractionThe mixture was then extracted into ethyl acetate (4×20 ml)
  4. dry with materialdried (MgSO4)
  5. customThe solvent was evaporated
  6. customthe residue chromatographed on silica gel

出典と根拠

ORDレコード
ord-dc748a3bf96d4ed99180ec254ab8785e
出典データセット
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05681833

反応ノート

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