Ethanol → Ethyl 3-Aminoisonicotinate

HRID 227584

反応式

HRID 227584 の反応式
[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]

参加物

5

反応物 4

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

生成物 1

HCID 2736365Ethyl 3-Aminoisonicotinate収率 87%

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-67d96eb2975649e3885db6bf1f096cfe
出典データセット
uspto-grants-2009_07
特許番号
US07560564B2

関連ノート

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