関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Citric Acid | HCID 311 | — |
| 反応物 | Ethyl formate | HCID 8025 | — |
| 反応物 | Ethyl 3-phenylpropionate | HCID 16237 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 2-benzyl-3-oxopropanoate | HCID 562571 | 86.9% |
反応手順
To a suspension solution containing 4.4 g of 60% NaH in 200 ml of THF, 17.8 g of ethyl 3-phenylpropionate and 8.2 g of ethyl formate were added dropwise under ice cool for one hour. Thereafter, the mixture was stirred at room temperature for 15 hours. Furthermore, 14 g of 60 % NaH and 25.9 g of ethyl formate were divided into three parts and each part was added separately. Afterwards, the solution mixture was stirred at room temperature for 15 hours. After a 10% citric acid solution was added to the resultant reaction solution, the reaction solution was extracted with ethyl acetate and the extract was concentrated under reduced pressure to obtain 32.4 g of a brown oily concentrate. The concentrate thus obtained was purified by silica gel column chromatography to obtain 17.9 g of the titled compound as a transparent oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07666659B2 |
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| 出典データセット | uspto-grants-2010_02 |
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| ORD ID | ord-072297d6388b42499252a23ee3c7cb95 |
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| 出典メモ | uspto-grants-2010_02 |
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