Methyl iodide → N-(1-methylimidazol-2-yl)benzylideneamine

HRID 741708노트

반응식

HRID 741708 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[N:6]=[CH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH3:14]C(C)([O-])C.[K+].CI>CN(C=O)C>[CH3:14][N:1]1[CH:5]=[CH:4][N:3]=[C:2]1[N:6]=[CH:7][C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 23665647Potassium tert-butoxideHCID 53795682N-[(1E)-phenylmethylidene]-1H-imidazol-2-amine

생성물 1

HCID 53843952N-(1-methylimidazol-2-yl)benzylideneamine수율 49.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

N-(2-imidazolyl)benzylideneamine (0.2 g) was dissolved in DMF (4 ml), and potassium t-butoxide (0.15 g) and methyl iodide (0.18 g) were added. The mixture was stirred at room temperature for 3 hours. The solvent was evaporated, and water was added. The mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried over magnesium sulfate, and the solvent was evaporated. The residue was purified by silica gel column chromatography (eluent: chloroform). The resulting crude crystals were recrystallized from diethyl ether--hexane to give the title compound (0.1 g, 49.9%) as pale yellow needles.

후처리

  1. customThe solvent was evaporated
  2. additionwater was added
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated brine
  5. dry with materialdried over magnesium sulfate
  6. customthe solvent was evaporated
  7. customThe residue was purified by silica gel column chromatography (eluent: chloroform)
  8. customThe resulting crude crystals were recrystallized from diethyl ether

출처 및 근거

ORD 기록
ord-4e1abe74d4f54f24aa0ee8eaf6f59d0b
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05552427

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