関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Phenylacetone | HCID 7678 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Phenyl-3-buten-2-one | HCID 324797 | — |
反応手順
1-Phenyl-propan-2-one (40.8 g) was dissolved in 200 ml of MeOH. Formaline (37%) (79 mL), piperidine (4 ml) and HOAc (4 ml) where added and de reaction was stirred for 3 h at 60° C. The reaction mixture was evaporated to dryness under reduced pressure. The residue was taken up in diethyl ether, and extracted with water. The organic layer was washed with 1M HCl, dried over MgSO4 and evaporated under reduced pressure to yield 36.3 g of a yellow liquid. 1H NMR (400 MHz, CDCl3) δ 2.41 (s, 3H), 5.87 (s, 1H), 6.18 (s, 1H), 7.24-7.40 (m, 5H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08722887B2 |
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| 出典データセット | uspto-grants-2014_05 |
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| ORD ID | ord-4cbc3d269f8e4475b49876afa34949c9 |
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| 出典メモ | uspto-grants-2014_05 |
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