関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Diethyl (2,6-dimethoxybenzylidene)malonate | HCID 12514881 | — |
| 触媒 | HCID 178418390 | HCID 178418390 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Diethyl (2,6-dimethoxybenzyl)malonate | HCID 54492584 | 74.5% |
反応手順
A mixture of 2.8 g of diethyl (2,6-dimethoxybenzylidene)malonate, 0.6 g of palladium-carbon, 50 ml of methanol and 50 ml of glacial acetic acid was stirred at 25° C. overnight. The solution was filtered and concentrated, and the residue was taken up in ethyl acetate and extracted with 20% NaHCO3 and some ice. Thereafter, the mixture was extracted with 1N, HCl, back-washed with saturated NaCl solution, the organic phase was dried and evaporated under reduced pressure. The crude product was distilled in a high vacuum at 170° C./0.6 mbar. 2.1 g of diethyl (2,6-dimethoxybenzyl)malonate were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05270313 |
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| 出典データセット | uspto-grants-1993_12 |
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| ORD ID | ord-c12ef67124014ed496644793feff3d58 |
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| 出典メモ | uspto-grants-1993_12 |
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