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Diethyl Ether → 2-[2-(4-Fluorophenyl)acetyl]4-methoxy-pyrazolidine-1-carboxylic acid benzyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 2-[2-(4-Fluorophenyl)acetyl]-4-hydroxypyrazolidine-1-carboxylic acid benzyl ester | HCID 20724744 | — |
| 触媒 | Silver(II) oxide | HCID 92152 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[2-(4-Fluorophenyl)acetyl]4-methoxy-pyrazolidine-1-carboxylic acid benzyl ester | HCID 20724745 | 97% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06849627B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-753ae2739ad741178e4c270cf4e13deb |
| 出典メモ | uspto-grants-2005_02 |