반응 #7763

반응 방정식

2-[2-(4-Fluorophenyl)acetyl]-4-hydroxy-pyrazolidine-1-carboxylic acid benzyl ester

Methyl iodide

ether

→

desired product

수율 97.0%

2-[2-(4-fluorophenyl)acetyl]-4-methoxy-pyrazolidine-1-carboxylic acid benzyl ester

수율 97.0%

용매

dimethylformamide

반응 조건

후처리

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

실험 절차

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.

출처