Methanol → Methyl 3-Hydroxy-2-pyridinecarboxylate

HRID 7148

반응식

HRID 7148 반응식
[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

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 134013-Hydroxypicolinic Acid

생성물 1

HCID 819341Methyl 3-Hydroxy-2-pyridinecarboxylate

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6f4859518ebb480b9bc417db7ce45ca2
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084155B2

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