Ethanol → N-Cycloheptyl-1-(2-fluorenyl)ethylamine

HRID 256627

反応式

HRID 256627 の反応式
[C:1]([C:4]1[CH:16]=[CH:15][C:14]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[CH2:7][C:6]=2[CH:5]=1)(=O)[CH3:2].[CH:17]1([NH2:24])[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.C(O)C.[BH4-].[Na+]>O>[CH:17]1([NH:24][CH:1]([C:4]2[CH:16]=[CH:15][C:14]3[C:13]4[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=4)[CH2:7][C:6]=3[CH:5]=2)[CH3:2])[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1

参加物

6

反応物 4

HCID 702EthanolHCID 2899CycloheptylamineHCID 699082-AcetylfluoreneHCID 4311764Sodium borohydride

生成物 1

HCID 19936135N-Cycloheptyl-1-(2-fluorenyl)ethylamine収率 25.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-Acetylfluorene (4.17 g, 20 mmol) and cycloheptylamine (2.38 g, 21 mmol) were heated together at 130° C. for 14 hrs and, then, distilled under reduced pressure. To the residue were added ethanol (20 ml) and sodium borohydride (0.76 g, 20 mmol) and the mixture was stirred at room temperature overnight. The mixture was then diluted with water (100 ml) and extracted with chloroform (80 ml×2 times). The organic layer was dried over anhydrous magnesium sulfate and concentrated. The residue was then purified by silica gel column chromatography to give 1.58 g of the amine compound.

後処理

  1. distillationdistilled under reduced pressure
  2. extractionextracted with chloroform (80 ml×2 times)
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was then purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-7dcfd16b782c4ba2929e912769308f27
出典データセット
uspto-grants-1993_11
特許番号
US05258405

関連ノート

読み込み中…