Reaktion #2336445

ord-5e247f958bba46a3bb0b5270b612bc84

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter 2 to 3 hours 1-diphenylmethyl-4-[(2-(4-methylphenyl)-5-methyl-1H-imidazol-4-yl)methyl]piperazine precipitated from the reaction mixture
  2. 2
    workup.WAITAfter having left the crystals
  3. 3
    Sonstigestanding at room temperature
  4. 4
    Sonstigethey were removed by filtration
  5. 5
    Sonstigerecrystallized from methanol
  6. 6
    Sonstigeto give the free base which melted at 220°-222° C.

Vorschrift

50 Grams (0.2 mol) of 2-(4-methylphenyl)-4-chloromethyl-5-methyl-1H-imidazole hydrochloride dissolved in 200 ml of a mixture of ethanol:water 6:4 were added dropwise to a refluxing solution of 55 grams (0.2 mol) of N-(diphenylmethyl)piperazine and 24 grams (0.6 mol) sodium hydroxide in 200 ml of a mixture of ethanol:water 6:4. After 2 to 3 hours 1-diphenylmethyl-4-[(2-(4-methylphenyl)-5-methyl-1H-imidazol-4-yl)methyl]piperazine precipitated from the reaction mixture. After having left the crystals standing at room temperature, they were removed by filtration and recrystallized from methanol to give the free base which melted at 220°-222° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05043447uspto-grants-1991_08