関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron tribromide | HCID 25134 | — |
| 反応物 | Benzaldehyde, 4-hydroxy-3-iodo-5-methoxy- | HCID 79499 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3,4-Dihydroxy-5-iodobenzaldehyde | HCID 14028211 | 66.2% |
反応手順
37.2 g of 5-iodo vanillin (commercial) and 360 ml of dichloromethane were mixed together under nitrogen and the mixture was cooled to 0° C. 135 ml of a molar solution of boron tribromide in dichloromethane were added and the mixture stood for 16 hours at ambient temperature and was then concentrated, cooled to 0° C. and acidified. The crystallized product was separated out, washed with water, dried and crystallized from an isopropanol--water mixture (1-2 by volume) to obtain 23.4 g of the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728828 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-23ad7b54403248708606eeee9fbf6470 |
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| 出典メモ | uspto-grants-1998_03 |
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