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

HRID 256627

반응식

HRID 256627 반응식
[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

참가 물질

6

반응물 4

HCID 702EthanolHCID 2899CycloheptylamineHCID 699082-AcetylfluoreneHCID 4311764Sodium borohydride

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7dcfd16b782c4ba2929e912769308f27
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258405

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