Hydroxyamine hydrochloride → 3-Cyano-2-hydroxy-5-methylbenzoic acid
反応式
[CH:1]([C:3]1[CH:11]=[C:10]([CH3:12])[CH:9]=[C:5]([C:6]([OH:8])=[O:7])[C:4]=1[OH:13])=O.Cl.[NH2:15]O>CN(C)C=O>[C:1]([C:3]1[CH:11]=[C:10]([CH3:12])[CH:9]=[C:5]([C:6]([OH:8])=[O:7])[C:4]=1[OH:13])#[N:15]参加物
4
実験手順
3-Formyl-5-methylsalicylic acid (3.6 g) was dissolved in dimethylformamide (20 ml) and treated with hydroxylamine hydrochloride (1.53 g). The mixture was heated at reflux for 10 minutes and then the solvent was removed in vacuo. The residue was treated with water (20 ml) and hydrochloric acid (2N; 10 ml). The precipitated solid was filtered off and recrystallized from aqueous ethanol to give 3-cyano-5-methylsalicylic acid (2.7 g), m.p. 193°-194° C.
後処理
- temperatureThe mixture was heated
- temperatureat reflux for 10 minutes
- customthe solvent was removed in vacuo
- additionThe residue was treated with water (20 ml) and hydrochloric acid (2N; 10 ml)
- filtrationThe precipitated solid was filtered off
- customrecrystallized from aqueous ethanol
出典と根拠
- ORDレコード
- ord-6bf09be2664f41b7aeee29e79df865ca
- 出典データセット
- uspto-grants-1979_03
- 特許番号
- US04146631
反応ノート
読み込み中…