반응 #93525

ord-fb2bddfe699b4d449664e8856f0077d0

반응 조건

온도
115°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the progress of the reaction by thin-layer chromatography on silica gel (MeOH: NaCl(1M), 92:8)
  2. 2
    기타At the completion of the reaction
  3. 3
    온도cool
  4. 4
    기타to obtain an oil
  5. 5
    기타Triturate the oil with petroleum ether until a solid
  6. 6
    기타precipitates
  7. 7
    기타Recrystallize the solid from MeOH/ acetone
  8. 8
    여과filter
  9. 9
    기타dry in vacuo

실험 절차

To 4.77 g (0.023 mole) 1-chloro-4-(4-chlorobutyl)benzene add 2.23 g (0.023 mole) 1,2-dimethyl-1H-imidazole. Stir the solution for three hours at about 115° C. Follow the progress of the reaction by thin-layer chromatography on silica gel (MeOH: NaCl(1M), 92:8). At the completion of the reaction, cool to obtain an oil. Triturate the oil with petroleum ether until a solid precipitates. Recrystallize the solid from MeOH/ acetone; filter and dry in vacuo to yield the title compound as a monohydrate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04613609uspto-grants-1986_09