関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Ethynylcyclohexane | HCID 70263 | — |
| 反応物 | HCID 178418443 | HCID 178418443 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3-Cyclohexylprop-2-yn-1-ol | HCID 316601 | — |
反応手順
To a solution of ethyl magnesium bromide (prepared from 2.5 g of magnesium turning and 11.3 g of bromoethane) in ether was added dropwise a solution of 10.2 g of cyclohexylacetylene in ether and the reaction mixture was refluxed for 2 hours. The reaction mixture was cooled to ambient temperature and anhydrous formaldehyde (prepared from the thermal decomposition of 50 g of paraformaldehyde for 20 minutes) was bubbled into the mixture. After cooling, the reaction was quenched with saturated ammonium chloride and extracted with ether (2×100 ml). The combined ether extracts were washed with brine, dried over magnesium sulfate and evaporated to yield the product which was distilled under high vacuum at 68°-74° C. to yield 6.4 g as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728694 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-d99b336bab874ba9a769f33bfde68ea1 |
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| 出典メモ | uspto-grants-1998_03 |
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