Hydrochloric Acid → 4-(1-Methyl-4,5-dihydro-1H-imidazol-2-yl)-phenylamine

HRID 2244962

반응식

HRID 2244962 반응식
[NH2:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#N)=[CH:4][CH:3]=1.Cl.[CH3:11][NH:12][CH2:13][CH2:14][NH2:15]>CO>[CH3:11][N:12]1[CH2:13][CH2:14][N:15]=[C:6]1[C:5]1[CH:8]=[CH:9][C:2]([NH2:1])=[CH:3][CH:4]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 8014N-MethylethylenediamineHCID 133964-Aminobenzonitrile

생성물 1

HCID 227288764-(1-Methyl-4,5-dihydro-1H-imidazol-2-yl)-phenylamine수율 49.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 4-aminobenzonitrile (5.1 g, 43 mmol) in dry methanol (60 mL) at 0 C, hydrogen chloride gas was bubbled through until saturation was reached. The mixture was then stirred at room temperature overnight. It was concentrated in vacuo. The residue was dissolved in dry methanol (60 mL). To the solution, N-methyl ethylenediamine (19 mL, 216 mmol) was added. The mixture was then heated to reflux for 3 h. After being cooled in fridge overnight, the precipitated product was collected by filtration, then was dried on vacuum to give white solids (3.7 g). MS 176.0 (M+H).

후처리

  1. concentrationIt was concentrated in vacuo
  2. dissolutionThe residue was dissolved in dry methanol (60 mL)
  3. temperatureThe mixture was then heated
  4. temperatureto reflux for 3 h
  5. temperatureAfter being cooled in fridge overnight
  6. filtrationthe precipitated product was collected by filtration
  7. customwas dried on vacuum

출처 및 근거

ORD 기록
ord-6fd288883ee34f8499d1fd52141b360a
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07678913B2

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