Hydrochloric Acid → Ethyl 5-aminopyridine-3-carboxylate

HRID 488453

반응식

HRID 488453 반응식
[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]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 3543165-Aminonicotinic Acid

생성물 1

HCID 910920Ethyl 5-aminopyridine-3-carboxylate

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-143667ca793a4c3d9c92b1bad47432ed
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06972297B2

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