参与物
| 角色 | 名称 | HCID | 投料 |
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| 反应物 | 海萝胶 | HCID 313 | — |
| 反应物 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 反应物 | 阿魏酸 | HCID 445858 | — |
| 溶剂 | Ethyl acetate hexane | HCID 21226206 | — |
| 产物 | 阿魏酸甲酯 | HCID 5357283 | — |
反应步骤
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%).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US05621009 |
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| 来源数据集 | uspto-grants-1997_04 |
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| ORD ID | ord-95b45af7e71e4a62a248194e8feab55d |
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| 来源说明 | uspto-grants-1997_04 |
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