参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 三溴化硼 | HCID 25134 | — |
| 反应物 | 5-氯香草醛 | HCID 29622 | — |
| 溶剂 | 二氯甲烷 | HCID 6344 | — |
| 产物 | 3-氯-4,5-二羟基苯甲醛 | HCID 2468182 | 77.3% |
反应步骤
37.2 g of commercial 5-chloro vanillin and 800 ml of dichloromethane were mixed together under nitrogen and cooled to 0° C. 300 ml of a molar solution of boron tribromide in dichloromethane are added and the mixture stood for one night at ambient temperature. It was concentrated, cooled again to 0° C. and acidified. The crystallized product was separated, washed with water, dried and crystallized from an isopropanol- water mixture (1-2 by volume) to obtain 26.6 g of the expected product melting at >260° C.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US05728828 |
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| 来源数据集 | uspto-grants-1998_03 |
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| ORD ID | ord-49d72313e0d6412c95d675c45339c241 |
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| 来源说明 | uspto-grants-1998_03 |
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