Hydroxyamine hydrochloride → 3-Cyano-2-hydroxy-5-methylbenzoic acid
반응식
[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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-6bf09be2664f41b7aeee29e79df865ca
- 출처 데이터셋
- uspto-grants-1979_03
- 특허 번호
- US04146631
반응 노트
불러오는 중…