تفاعل #50971

ord-753ae2739ad741178e4c270cf4e13deb

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGThe mixture is stirred vigorously at room temperature
  2. 2
    ترشيحfiltered through a pad of Celite
  3. 3
    غسيلThe filtrate is washed with water (2×150 mL) and brine (150 mL)
  4. 4
    تجفيفdried over sodium sulfate
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated in vacuo

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06849627B2uspto-grants-2005_02