Cycloheptylamine → N-Cycloheptyl-[(2-phenanthrenyl)methyl]amine

HRID 256623

반응식

HRID 256623 반응식
[CH3:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH:6]=[CH:5][C:4]=2[CH:3]=1.BrN1C(=O)CCC1=O.[CH:24]1([NH2:31])[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH:24]1([NH:31][CH2:1][C:2]2[CH:15]=[CH:14][C:13]3[C:12]4[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=4)[CH:6]=[CH:5][C:4]=3[CH:3]=2)[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1

참가 물질

6

반응물 4

HCID 2899CycloheptylamineHCID 11430Potassium CarbonateHCID 173212-MethylphenanthreneHCID 67184N-bromobutanimide

생성물 1

HCID 15284290N-Cycloheptyl-[(2-phenanthrenyl)methyl]amine수율 66.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2-Methylphenanthrene (2.00 g, 10.4 mmol) was brominated with N-bromosuccinimide (2.05 g, 11.5 mmol) and the product compound was added gradually to a suspension of cycloheptylamine (2.38 g, 21.0 mmol) and potassium carbonate (2.90 g, 21.0 mmol) in dimethylformamide (20 ml) with ice-cooling. The mixture was then stirred at room temperature for 16 hrs and, then, filtered and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 2.11 g of a viscous liquid.

후처리

  1. temperaturecooling
  2. filtrationfiltered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-450d9398ff814e4c9fe9af5967e21e18
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258405

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