関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Diazomethane | HCID 9550 | — |
| 反応物 | 4,4-Diethoxybut-1-ene | HCID 256426 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-(2,2-Diethoxyethyl)cyclopropane | HCID 23264569 | — |
反応手順
Diazomethane (6.17 g, 147 mmol) was added dropwise to 3.02 g (21 mmol) of 3-butenal diethyl acetal in 10 ml of dry ether with intensive stirring at 0° C. Then 70 mg (0.312 mmol) of palladium (II) acetate in 50 ml of dry ether was added all at once. Then stirring at 0° C. continued until the evolution of N2 ceased (10 min.). The ether was distilled off to the reduced volume of the reaction mixture ca 10 ml. The precipitate was filtered off on a fritted glass funnel and the filtrate evaporated. The crude product (2.57 g) contained 97% of the title compound (GC) and was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06114365 |
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| 出典データセット | uspto-grants-2000_09 |
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| ORD ID | ord-ac349e32008f4c8e8140cd83140d9543 |
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| 出典メモ | uspto-grants-2000_09 |
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