関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propanal | HCID 527 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Ethyl dichloroacetate | HCID 10808 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 生成物 | Ethyl 3-chloro-2-oxopentanoate | HCID 13719444 | — |
反応手順
Sodium ethoxide (0.68 g, 9.94 mmol) was added portionwise to a mixture of ethyldichloroacetate (1.22 ml, 9.94 mmol) and diethyl ether (10 ml) under ice-water cooling and the resulting mixture was stirred at 0° C. for 30 minutes. Propionaldehyde (0.79 ml, 10.93 mmol) was then added and the reaction mixture allowed to warm to room temperature slowly and stirring continued for 72 hours. The reaction mixture was then poured onto water (10 ml) and extracted with diethyl ether (2×15 ml). The organic layers were combined, dried over magnesium sulfate, and concentrated in vacuo to yield crude 3-chloro-2-oxo-pentanoic acid ethyl ester (1.8 g) which was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07700634B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-5308c45182cf4ab583db80ba46a4ea2d |
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| 出典メモ | uspto-grants-2010_04 |
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