Acetic Acid → 2-Methyl-3-(4-pyridin-3-yl-imidazol-1-yl)-propioaldehyde

HRID 432570노트

반응식

HRID 432570 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:8]=[CH:9][NH:10][CH:11]=2)[CH:2]=1.C(O)(=O)C.[O:16]=[CH:17][C:18](=[CH2:20])[CH3:19]>C1COCC1>[CH3:19][CH:18]([CH2:20][N:10]1[CH:11]=[C:7]([C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)[N:8]=[CH:9]1)[CH:17]=[O:16]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 6562Methacrolein2회HCID 178420772HCID 178420772, 화합물

생성물 1

HCID 187597712-Methyl-3-(4-pyridin-3-yl-imidazol-1-yl)-propioaldehyde

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 4-pyridin-3-yl-imidazole (8.5 g) in THF (293 mL) was added acetic acid (16.8 mL) and methacrolein (9.7 mL) and the resulting solution was heated under gentle reflux for 24 hours. Another 9.7 mL methacrolein was added and the solution was heated under reflux for another 24 hours. THF was then removed in vacuo and the residue was purified on a Flash 75 long column eluting with MeOH—CH2Cl2 to give the title compound as slightly yellow oil.

후처리

  1. temperaturethe resulting solution was heated
  2. temperatureunder gentle reflux for 24 hours
  3. temperaturethe solution was heated
  4. temperatureunder reflux for another 24 hours
  5. customTHF was then removed in vacuo
  6. customthe residue was purified on a Flash 75 long column
  7. washeluting with MeOH—CH2Cl2

출처 및 근거

ORD 기록
ord-4d2c8b545199473fad18556ba2df287a
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06664238B1

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