化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → 2-[2-(4-Fluorophenyl)acetyl]4-methylene-pyrazolidine-1-carboxylic acid benzyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Fluorophenylacetyl chloride | HCID 3744988 | — |
| 反応物 | Benzyl 4-methylidenepyrazolidine-1-carboxylate | HCID 12970153 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Water methylene chloride | HCID 21908982 | — |
| 生成物 | 2-[2-(4-Fluorophenyl)acetyl]4-methylene-pyrazolidine-1-carboxylic acid benzyl ester | HCID 12970154 | 62% |
反応手順
Sodium hydroxide (0.12 g, 3 mmol) is dissolved in a 1:2 water/methylene chloride solution (30 mL) with rapid stirring followed by the addition of 4-methylene-pyrazolidine-1-carboxylic acid 1-benzyl ester, 9, (0.62 g, 2.8 mmol) at room temperature. (4-Fluorophenyl)acetyl chloride (0.39 mL, 4.2 mmol) is added and the reaction is allowed to stir for 18 hours after which time the reaction mixture is diluted with water (10 mL) and the layers allowed to separate. The aqueous layer is extracted with methylene chloride, the organic layers combined, dried, and filtered. Concentration in vacuo affords the crude product which is purified over silica (1:3 ethyl acetate/hexane) to provide 0.54 g (62% yield) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087615B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-500db76911fe4a4ead497cd52689022e |
| 出典メモ | uspto-grants-2006_08 |