関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 4-Pyridinecarboxaldehyde | HCID 13389 | — |
| 反応物 | 1-Bromo-2-(dimethoxymethyl)-4,5-dimethoxybenzene | HCID 11077146 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3,4-Dimethoxy-6-(4-pyridyl) hydroxymethylbenzaldehyde dimethylacetal | HCID 22007378 | — |
反応手順
A solution of 6-bromo-3,4-dimethoxybenzaldehyde dimethyl acetal (20 ml) in tetrahydrofuran (100 ml) is cooled to -60° C., and thereto is added dropwise a 1.6 M solution of n-butyl lithium in hexane (45.1 ml) over a period of 20 minutes under nitrogen atmosphere. The mixture is reacted at the same temperature for 30 minutes, and thereto is added dropwise a solution of 4-formylpyridine (7.36 g) in tetrahydrofuran (50 ml) over a period of 20 minutes. The reaction mixture is reacted for one hour, and thereto are added water and ethyl acetate (200 ml). The ethyl acetate layer is separated, washed, dried, and concentrated under reduced pressure to remove the ethyl acetate to give 3,4-dimethoxy-6-(4-pyridyl)hydroxymethylbenzaldehyde dimethyl acetal (15.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06005106 |
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| 出典データセット | uspto-grants-1999_12 |
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| ORD ID | ord-8093544aa6e74d0085035f2ef33c5224 |
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| 出典メモ | uspto-grants-1999_12 |
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