3-Hydroxyanthranilic Acid → Anthranilic acid, 3-hydroxy-, methyl ester

HRID 380520

反応式

HRID 380520 の反応式
[NH2:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl.[CH3:13]O>>[CH3:13][O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][CH:9]=[C:10]([OH:11])[C:2]=1[NH2:1]

参加物

4

反応物 3

HCID 863-Hydroxyanthranilic AcidHCID 313Hydrochloric AcidHCID 887Methanol

生成物 1

HCID 205248Anthranilic acid, 3-hydroxy-, methyl ester

実験手順

To a solution of 2 g (13.1 mmol) of 2-amino-3-hydroxybenzoic acid in 60 mL of CH3OH at 0° C. was bubbled HCl gas until the solution was saturated. The reaction was heated at reflux for 12 h. The reaction mixture was concentrated and dissolved in 30 mL of water. The solution was neutralized with sat'd NaHCO3 solution and extracted with EtOAc. The organic fractions were dried over MgSO4, filtered and the filtrate was concentrated to give 1.8 g of the title compound as a brown solid.

後処理

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 12 h
  3. concentrationThe reaction mixture was concentrated
  4. dissolutiondissolved in 30 mL of water
  5. extractionextracted with EtOAc
  6. dry with materialThe organic fractions were dried over MgSO4
  7. filtrationfiltered
  8. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-705586a0a1d6491bae150b800fb4e115
出典データセット
uspto-grants-2001_10
特許番号
US06303593B1

関連ノート

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