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Hydrogen Bromide → 2,3-Dihydroxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | o-Vanillin | HCID 8991 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2,3-Dihydroxybenzaldehyde | HCID 90579 | 70.2% |
反応手順
152.0 g (1.0 mol) of o-vanillin and 200 ml of azeotropic hydrobromic acid (47.5% strength) are stirred under reflux in 500 ml of glacial acetic acid for 2.5 hours. The acid mixture is then distilled off and the residue is subjected to fractional vacuum distillation. The redistilled fraction having a boiling point of 120°-125° C./12 mbar is purified by recrystallisation from 1 l of heptane (hexane is also possible and is recovered). 97 g (70% of theory) of 2,3-dihydroxybenzaldehyde of melting point 105°-107° C. are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05420308 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-8e7891df21cc4ed39de4bc1a4c84a2c9 |
| 出典メモ | uspto-grants-1995_05 |