関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl formate | HCID 8025 | — |
| 反応物 | Diethyl Succinate | HCID 31249 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1,4-Diethyl 2-formylbutanedioate | HCID 231500 | 107.2% |
反応手順
To a suspension of sodium (333 mg, 14 mmol, 1.2 eq) in diethyl ether (7 mL) were added succinic acid diethyl ester (2.1 g, 12 mmol, 1 eq) and formic acid ethyl ester (1.7 mL, 20 mmol, 1.7 eq). The mixture was stirred at 40° C. for 5 h. Water (10 mL) was added and the aqueous layer was washed with diethyl ether (2×10 mL). The aqueous layer was then acidified with a 6N solution of hydrochloric acid and extracted with diethyl ether (3×10 mL). The organic layers were dried over magnesium sulfate, filtered and evaporated in vacuo to afford the expected compound as orange oil (2.6 g, quant. yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434745B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-2af018deacdc422e955be1e741a90177 |
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| 出典メモ | uspto-grants-2016_09 |
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