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

HRID 2174685

反応式

HRID 2174685 の反応式
[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]

参加物

5

反応物 4

HCID 887MethanolHCID 1066Quinolinic AcidHCID 1118Sulfuric AcidHCID 10340Sodium Carbonate

生成物 1

HCID 690582,3-Dimethyl 2,3-pyridinedicarboxylate

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3b19b6432f254ab399d3b17d25803d23
出典データセット
uspto-grants-2015_06
特許番号
US09062033B2

関連ノート

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