Methanol → Methyl 3-Hydroxy-2-pyridinecarboxylate

HRID 7148

反応式

HRID 7148 の反応式
[OH:1][C:2]1[C:3]([C:8]([OH:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.OS(O)(=O)=O.[CH3:16]O>>[CH3:16][O:9][C:8](=[O:10])[C:3]1[C:2]([OH:1])=[CH:7][CH:6]=[CH:5][N:4]=1

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 134013-Hydroxypicolinic Acid

生成物 1

HCID 819341Methyl 3-Hydroxy-2-pyridinecarboxylate

実験手順

To a stirred solution of 3-hydroxypicolinic acid (0.7122 g, 5.1 mmol) in CH3OH (32 mL) at room temperature was added concentrated H2SO4 (4 mL). The mixture was heated to reflux for 18 hrs then concentrated. The residue was diluted with saturated aqueous Na2CO3 (45 mL) and extracted with CH2Cl2 (4×30 mL). The combined organic phases were dried (Na2SO4) and concentrated to give 0.73 g 3-hydroxypicolinic acid methyl ester as a white powder.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 18 hrs
  3. concentrationthen concentrated
  4. additionThe residue was diluted with saturated aqueous Na2CO3 (45 mL)
  5. extractionextracted with CH2Cl2 (4×30 mL)
  6. dry with materialThe combined organic phases were dried (Na2SO4)
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-6f4859518ebb480b9bc417db7ce45ca2
出典データセット
uspto-grants-2006_08
特許番号
US07084155B2

関連ノート

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