تفاعل #573378

ord-0be350ce7e334f58a5cbfa9c04cf2ce7

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter evaporation of the solvent
  2. 2
    workup.ADDITIONthe residue was diluted with water
  3. 3
    استخلاصextracted three times with chloroform
  4. 4
    غسيلThe organic layer was washed with brine
  5. 5
    تجفيفdried over anhydrous magnesium sulfate
  6. 6
    أخرىevaporated in vacuo
  7. 7
    أخرىPurification of the residue with silica gel column chromatography (15% methanol-chloroform)
  8. 8
    أخرىfollowed by recrystallization from methanol

الإجراء التجريبي

A solution of 8,9-dihydro-7-[(hydroxy)(1-trityl-1H-imidazol-2-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one (376 mg) in acetic acid (15 ml) and water (5 ml) was stirred at 60° C. for 2.5 hours. After evaporation of the solvent, the residue was diluted with water, neutralized with an aqueous solution of sodium hydrogencarbonate, and extracted three times with chloroform. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. Purification of the residue with silica gel column chromatography (15% methanol-chloroform), followed by recrystallization from methanol, gave 8,9-dihydro-7-[(hydroxy)(1H-imidazol-2-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one (148 mg).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05290785uspto-grants-1994_03