反应 #48567

ord-dcb2307e136e4b1189f2da3b32c6ceb2

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The reaction mixture was filtered through Celite®
  2. 2
    workup.ADDITIONdiluted with ethyl acetate
  3. 3
    洗涤washed with brine
  4. 4
    干燥dried (MgSO4)
  5. 5
    其他evaporated

实验过程

To a solution of 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (200 mg; 1 mmol) and cyclohexanone (107 mg; 1.1 mmol) in dichloromethane (10 ml) were added 3 Å molecular sieves (1 g) and sodium triacetoxyborohydride (315 mg; 1.5 mmol), and the mixture was then stirred at room temperature over the weekend. The reaction mixture was filtered through Celite®, diluted with ethyl acetate, washed with brine, dried (MgSO4) and evaporated to give the 48 mg of the product as a grey gum. (LC/MS: Rt 2.95, [M+H]+ 285).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07745638B2uspto-grants-2010_06