Methanol → 2,3-Dimethyl 2,3-pyridinedicarboxylate

HRID 2174685

Reaktionsgleichung

Reaktionsgleichung von HRID 2174685
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([OH:9])=[O:8])[C:2]=1[C:10]([OH:12])=O.S(=O)(=O)(O)O.[C:18](=O)([O-])[O-].[Na+].[Na+].[CH3:24][OH:25]>>[CH3:24][O:25][C:10]([C:2]1[C:3]([C:7]([O:9][CH3:18])=[O:8])=[CH:4][CH:5]=[CH:6][N:1]=1)=[O:12]

Komponenten

5

Versuchsvorschrift

To a solution of pyridine-2,3-dicarboxylic acid (50.0 g, 0.299 mol) in methanol (500 ml) was added con. sulfuric acid (20 ml). After heated to reflux for 24 hours, the mixture was basified with saturate sodium carbonate solution until pH=8 and then extracted with ethyl acetate. The combined extracts were washed with brine, dried over magnesium sulphate, filtered and evaporated to give D78 (45.7 g) as a white solid.

Aufarbeitung

  1. temperatureAfter heated
  2. temperatureto reflux for 24 hours
  3. extractionextracted with ethyl acetate
  4. washThe combined extracts were washed with brine
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated
  8. customto give D78 (45.7 g) as a white solid

Quellen und Nachweise

ORD-Eintrag
ord-3b19b6432f254ab399d3b17d25803d23
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09062033B2

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