Sulfuric Acid → Dimethyl pyridine-3,5-dicarboxylate

HRID 1092185

반응식

HRID 1092185 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 78339Dimethyl pyridine-3,5-dicarboxylate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e396cb8fdfe14eef972433d8f391636a
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129411B2

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