関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | 2-Cyclohexylacetaldehyde | HCID 316627 | — |
| 生成物 | 2-Cyclohexylprop-2-en-1-al | HCID 12577070 | 81% |
反応手順
Successively, sulfuric acid 62% (79.4 g, 0.5 mol), aqueous formaldehyde 35% (82 g, 1.0 mol) and cyclohexyl acetaldehyde (100.8 g, 0.8 mol) were added slowly to diethylamine (73 g, 1.0 mol) at 0° C. After stirring at 80° C. overnight, the reaction mixture was extracted with MTBE. The combined organic phases were washed with H2O until neutral pH was achieved, dried (MgSO4) and concentrated in vacuo. The crude product was distilled under reduced pressure using a Widmer column (10 Torr, 80° C.) yielding 89.5 g (81%) of pure product as colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06184419B2 |
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| 出典データセット | uspto-grants-2001_02 |
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| ORD ID | ord-7a4e627e30f7477b81179cf836b5d1b1 |
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| 出典メモ | uspto-grants-2001_02 |
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