تفاعل #75147

ord-053899e364874c94ba6b10e86ce639cd

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةrefluxed overnight
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    ترشيحthe precipitated product is filtered off
  4. 4
    أخرىtriturated twice
  5. 5
    workup.ADDITIONfirst in a boiling mixture of 4-methyl-2-pentanone and 2-propanol
  6. 6
    ترشيحIt is filtered off again
  7. 7
    أخرىcrystallized from a mixture of N,N-dimethylformamide and water

الإجراء التجريبي

A mixture of 4.6 parts of 1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one, 5 parts of 1-(p-fluorophenyl)-1,3,8-triazaspiro[4,5]decan-4-one, 10 parts of sodium carbonate, 0.2 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. After cooling, the precipitated product is filtered off and triturated twice: first in a boiling mixture of 4-methyl-2-pentanone and 2-propanol and then in boiling methanol. It is filtered off again and crystallized from a mixture of N,N-dimethylformamide and water, yielding 4.5 parts of 8-[3-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)propyl]-1-(4-fluorophenyl)-1,3,8-triazaspiro-[4,5]-decan-4-one; mp. 215.4° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04175129uspto-grants-1979_11