関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron tribromide | HCID 25134 | — |
| 反応物 | 3-Chloro-4-hydroxy-5-methoxybenzaldehyde | HCID 29622 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Chloro-4,5-dihydroxybenzaldehyde | HCID 2468182 | 77.3% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06313305B1 |
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| 出典データセット | uspto-grants-2001_11 |
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| ORD ID | ord-1629714fd8b945d083be2677196e446f |
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| 出典メモ | uspto-grants-2001_11 |
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