Reaktion #1467538

ord-0cbe0d902f64453593f0f20d90ac897e

Reaktionsbedingungen

Temperatur
115°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe progress of the reaction by thin-layer chromatography on silica gel (MEOH:NaCL(1M), 92:8)
  2. 2
    SonstigeAt the completion of the reaction
  3. 3
    Temperaturcool
  4. 4
    Sonstigeto obtain an oil
  5. 5
    SonstigeTriturate the oil with petroleum ether until a solid
  6. 6
    Sonstigeprecipitates
  7. 7
    SonstigeRecrystallize the solid from MeOH/acetone
  8. 8
    Filtrationfilter
  9. 9
    Sonstigedry in vacuo

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04581370uspto-grants-1986_04