Hydrogen Bromide → 2,3-Dihydroxybenzaldehyde
反応式
[O:1]=[CH:2][C:3]1[CH:11]=[CH:10][CH:9]=[C:6]([O:7]C)[C:4]=1[OH:5].Br>C(O)(=O)C>[OH:5][C:4]1[C:6]([OH:7])=[CH:9][CH:10]=[CH:11][C:3]=1[CH:2]=[O:1]参加物
4
実験手順
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.
後処理
- distillationThe acid mixture is then distilled off
- distillationthe residue is subjected to fractional vacuum distillation
- customis purified by recrystallisation from 1 l of heptane (hexane
- customis recovered)
出典と根拠
- ORDレコード
- ord-8e7891df21cc4ed39de4bc1a4c84a2c9
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05420308
反応ノート
読み込み中…