関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Ferulic Acid | HCID 445858 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | Methyl Ferulate | HCID 5357283 | — |
反応手順
Ferulic acid (4.85 g) and then methyl alcohol (50 ml) containing hydrogen chloride (4%) were placed in an egg-plant type flask (200 ml), and heated under reflux for 1 hour. The disappearance of the starting material was confirmed by thin layer chromatography (TLC: n-hexane/ethyl acetate=2/1), then the solvent was evaporated under reduced pressure by a rotary evaporator. Benzene was added to the residue, and then, the solvent was again evaporated by a rotary evaporator to obtain the crude product. The resulting crude product was separated and purified by silica gel column chromatography (diameter=5.5×7.0 cm; 60 g; n-hexane/ethyl acetate=2/1) to obtain the above-identified compound. The product was crystallized from n-hexane to obtain a white crystal (5.09 g; 97.9%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05621009 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-95b45af7e71e4a62a248194e8feab55d |
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| 出典メモ | uspto-grants-1997_04 |
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