تفاعل #2829

ord-d4473f302a7441cbb178c086184f7270

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    ترشيحthe solution was filtered through celite 545
  3. 3
    أخرىto remove the catalyst
  4. 4
    أخرىThe solvent was evaporated under reduced pressure
  5. 5
    أخرىThe residue was purified by silica gel column chromatography (Kieselgel 60=20 g, ethyl acetate)

الإجراء التجريبي

The compound ([5]-(54)-75) (700 mg) prepared in Example 62 was dissolved in ethanol (35 ml). After the solution was heated to 50° C., a suspension of 10% Pd/C (70 mg) in ethanol was added, and hydrazine monohydrate (0.35 ml) was added to the solution. The solution was stirred at 50° C. for 30 minutes. After the reaction was completed, the solution was filtered through celite 545 to remove the catalyst. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (Kieselgel 60=20 g, ethyl acetate) to obtain the above-captioned compound ([5]-(55)-75) (631 mg) as colorless oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05731310uspto-grants-1998_03