Sulfuric Acid → HCID 22649192、化合物

HRID 393244ノート

反応式

HRID 393244 の反応式
[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

  1. temperatureThe mixture was cooled to ambient temperature
  2. additionpoured
  3. customonto crushed ice
  4. filtrationThe resultant solid was filtered off
  5. washwashed well with water
  6. 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…