反应 #2829

ord-d4473f302a7441cbb178c086184f7270

反应条件

温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05731310uspto-grants-1998_03