反应 #7763

ord-655bf75cb9f346c6bda87fc87af5a863

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGThe mixture is stirred vigorously at room temperature
  2. 2
    过滤filtered through a pad of Celite
  3. 3
    洗涤The filtrate is washed with water (2×150 mL) and brine (150 mL)
  4. 4
    干燥dried over sodium sulfate
  5. 5
    过滤filtered
  6. 6
    浓缩concentrated in vacuo

实验过程

2-[2-(4-Fluorophenyl)acetyl]-4-hydroxy-pyrazolidine-1-carboxylic acid benzyl ester, 28, (2.55 g, 7.91 mmol) is dissolved in dimethylformamide (40 mL). Methyl iodide (1.97 mL, 31.6 mmol) is added followed by silver oxide (3.67 g, 15.8 mmol). The flask is cover with foil and stirred overnight in the absence of light. The reaction mixture is poured into ether (150 mL). The mixture is stirred vigorously at room temperature and filtered through a pad of Celite. The filtrate is washed with water (2×150 mL) and brine (150 mL), dried over sodium sulfate, filtered and concentrated in vacuo to afford 2.58 g (97% yield) of the desired product as a yellow, clear oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07087615B2uspto-grants-2006_08