تفاعل #83239

ord-e4e18157eb9541c580754e8c4895a5e7

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was refluxed for 1 hour
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    أخرىthe reaction mixture was quenched with an aqueous saturated ammonium chloride solution
  4. 4
    استخلاصextracted with ethyl acetate
  5. 5
    غسيلThe extracts were washed with brine
  6. 6
    أخرىdried
  7. 7
    تركيزconcentrated in vacuo
  8. 8
    أخرىThe residue was crystallized from ethanol

الإجراء التجريبي

To a mixture of 4,7-dihydro-6-ethoxycarbonyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)-7-oxopyrazolo[1,5-a]pyrimidine (100 mg) in tetrahydrofuran (4 ml) was added lithium borohydride (2 mole in tetrahydrofuran, 0.26 ml) at room temperature and the mixture was refluxed for 1 hour. After cooling, the reaction mixture was quenched with an aqueous saturated ammonium chloride solution and extracted with ethyl acetate. The extracts were washed with brine, dried and concentrated in vacuo. The residue was crystallized from ethanol to give 6-ethoxycarbonyl-2-(4-fluorophenyl)-7-oxo-3-(pyridin-4-yl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine (40 mg).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05624931uspto-grants-1997_04