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

HRID 1432538노트

반응식

HRID 1432538 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-3a4b59b235d44c52afc14410ee8fee29
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612089B2

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