Ethanol → Ethyl 3-Aminoisonicotinate

HRID 227584

반응식

HRID 227584 반응식
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]([OH:10])=[O:9].S(=O)(=O)(O)O.[NH4+].[OH-].[CH2:18](O)[CH3:19]>>[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]([O:10][CH2:18][CH3:19])=[O:9]

참가 물질

5

반응물 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 14923Ammonium HydroxideHCID 4595313-Aminoisonicotinic acid

생성물 1

HCID 2736365Ethyl 3-Aminoisonicotinate수율 87%

실험 절차

To a solution of 1 g (7.25 mmol) of 3-amino-4-pyridinecarboxylic acid in 5 mL of ethyl alcohol was added 2 mL of sulfuric acid. The mixture was warmed under reflux for 2 h. It was cooled and basified with conc. NH4OH solution to pH=8. The resulting solution was extracted with ethyl acetate and the organic layer was washed with brine and water, dried (MgSO4) and concentrated in vacuo to give 1.04 g of the title compound as a white solid (87%).

후처리

  1. temperatureThe mixture was warmed
  2. temperatureunder reflux for 2 h
  3. temperatureIt was cooled
  4. extractionThe resulting solution was extracted with ethyl acetate
  5. washthe organic layer was washed with brine and water
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-67d96eb2975649e3885db6bf1f096cfe
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560564B2

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