Sulfuric Acid → Dimethyl pyridine-3,5-dicarboxylate

HRID 1092185

反応式

HRID 1092185 の反応式
[N:1]1[CH:6]=[C:5]([C:7]([OH:9])=[O:8])[CH:4]=C(C(O)=O)[CH:2]=1.OS(O)(=O)=O.[C:18]([O:21][CH2:22]C)(=[O:20])[CH3:19].[CH3:24]CCCCC>CO>[CH3:24][O:9][C:7]([C:5]1[CH:6]=[N:1][CH:2]=[C:19]([C:18]([O:21][CH3:22])=[O:20])[CH:4]=1)=[O:8]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 103663,5-Pyridinedicarboxylic acidHCID 21226206Ethyl acetate hexane

生成物 1

HCID 78339Dimethyl pyridine-3,5-dicarboxylate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3,5-Pyridinedicarboxylic acid (1.5 g, 63 mmol) and conc. H2SO4 (0.9 mL) in MeOH (15 mL) are heated in a microwave oven at 120° C. for 2 h. The solvent is evaporated to give a residue with is partitioned between ethyl acetate and sat. aq. NaHCO3. The organic phase is washed with brine, dried over Na2SO4, filtered and evaporated to give a light yellow solid. MS (LC-MS): 196 [M+H]+ TLC, Rf (ethyl acetate/hexane 1:1)=0.56.

後処理

  1. customThe solvent is evaporated
  2. customto give a residue
  3. customwith is partitioned between ethyl acetate and sat. aq. NaHCO3
  4. washThe organic phase is washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated
  8. customto give a light yellow solid

出典と根拠

ORDレコード
ord-e396cb8fdfe14eef972433d8f391636a
出典データセット
uspto-grants-2012_03
特許番号
US08129411B2

関連ノート

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