Hydrochloric Acid → Ethyl 5-aminopyridine-3-carboxylate

HRID 488453

反応式

HRID 488453 の反応式
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].Cl.[CH2:12](O)[CH3:13]>>[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([O:9][CH2:12][CH3:13])=[O:8]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 3543165-Aminonicotinic Acid

生成物 1

HCID 910920Ethyl 5-aminopyridine-3-carboxylate

実験手順

5-Aminonicotinic acid (2.2 g) (Bachman and Micucci, J. Amer. Chem. Soc. 70 (1948) 2381) in ethanol (20 ml) was ice-cooled, saturated with HCl gas and refluxed 4 hours. The mixture was concentrated to low volume and partitioned between EtOAc (100 ml) and saturated NaHCO3 solution (100 ml). The organic phase was washed with further aqueous NaHCO3, dried and evaporated to leave the title compound as a white solid (1.34 g). M.S. (+ve ion chemical ionisation) m/z 167 (MH+,100%).

後処理

  1. temperaturerefluxed 4 hours
  2. concentrationThe mixture was concentrated to low volume
  3. custompartitioned between EtOAc (100 ml) and saturated NaHCO3 solution (100 ml)
  4. washThe organic phase was washed with further aqueous NaHCO3
  5. customdried
  6. customevaporated

出典と根拠

ORDレコード
ord-143667ca793a4c3d9c92b1bad47432ed
出典データセット
uspto-grants-2005_12
特許番号
US06972297B2

関連ノート

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