Hydrochloric Acid → Methyl 5-amino-2-hydroxybenzoate

HRID 85350

反応式

HRID 85350 の反応式
Cl.[NH2:2][C:3]1[CH:4]=[CH:5][C:6]([OH:12])=[C:7]([CH:11]=1)[C:8]([OH:10])=[O:9].[CH3:13]O>>[NH2:2][C:3]1[CH:4]=[CH:5][C:6]([OH:12])=[C:7]([CH:11]=1)[C:8]([O:10][CH3:13])=[O:9]

参加物

4

実験手順

To a solution of saturated HCl in CH3OH (20 mL) at RT was slowly added 5-amino-2-hydroxybenzoic acid (2 g, 13.06 mmol). The resulting mixture was stirred at (RT, 16 h) and then heated (reflux, 24 h). The mixture was cooled and the solvent was removed under reduced pressure. The residue was diluted with EtOAc (50 mL) and washed with saturated aqueous NaHCO3. The organic solution was dried over MgSO4, filtered, concentrated under reduced pressure to afford methyl 5-amino-2-hydroxybenzoate as a pale yellow solid (1.72 g, 78.5%). Mass calculated for C8H9NO3=167.16; found: [M+H]+=168.2.

後処理

  1. customat RT
  2. temperatureheated
  3. temperature(reflux, 24 h)
  4. temperatureThe mixture was cooled
  5. customthe solvent was removed under reduced pressure
  6. additionThe residue was diluted with EtOAc (50 mL)
  7. washwashed with saturated aqueous NaHCO3
  8. dry with materialThe organic solution was dried over MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-8441a8b98d8d41c687b29e7f6848f3fe
出典データセット
uspto-grants-2014_09
特許番号
US08846972B2

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