関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 3-Acetylbenzonitrile | HCID 80222 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3-(2-Methyl-1,3-dioxolan-2-yl)benzonitrile | HCID 10559546 | 76% |
反応手順
To the mixture of ethylene glycol (0.22 mL, 4 mmol), 3-acetylbenzonitrile 18 (300 mg, 2.04 mmol) and benzene (10 mL) in a Dean-Stark apparatus was added a catalytic amount of p-TSA (0.1 equiv). The reaction mixture was heated at 110° C. for 4 h. The benzene was removed under reduced pressure and the residue was purified by column chromatography using ethylacetate-hexane as an eluent to give 19 (293 mg, 76%). 1H NMR (CDCl3, 400 MHz) δ 2.62 (s, 4H), 7.59 (t, J=7.6 Hz, 1H), 7.82 (d, J=7.6 Hz, 1H)), 8.15 (d, J=8 Hz, 1H), 8.21 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09447134B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-ac30645f01914ab68e8cb78b3f297fff |
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| 出典メモ | uspto-grants-2016_09 |
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