Sulfuric Acid → HCID 22649192、化合物
反応式
[NH2:1][C:2]1[C:11]([C:12]#[N:13])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([OH:14])[CH:3]=1.S(=O)(=O)(O)[OH:16]>>[NH2:1][C:2]1[C:11]([C:12](=[O:16])[NH2:13])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([OH:14])[CH:3]=1参加物
3
反応条件
- 温度
- 80 °C
実験手順
Methyl 4-amino-5-cyano-2-hydroxybenzoate (J. Chem. Soc. Perkin I. 1979, 677; 4 g) was added to stirred concentrated sulphuric acid (6 ml) and the mixture was heated to 80° C. for 30 minutes. The mixture was cooled to ambient temperature and poured onto crushed ice. The resultant solid was filtered off, washed well with water and dried to give methyl 4-amino-5-carbamoyl-2-hydroxybenzoate (2.8 g); NMR Spectrum: (DMSOd6) 3.83 (s, 3H), 6.1 (s, 1H), 6.75 (br m, 2H), 8.08 (s, 1H).
後処理
- temperatureThe mixture was cooled to ambient temperature
- additionpoured
- customonto crushed ice
- filtrationThe resultant solid was filtered off
- washwashed well with water
- customdried
出典と根拠
- ORDレコード
- ord-d5a0c989d63048798b83b9af9e2dfab8
- 出典データセット
- uspto-grants-2004_10
- 特許番号
- US06806274B1
反応ノート
読み込み中…