Hydrochloric Acid → 2-(1H-pyrazol-1-yl)pyridine

HRID 2099499노트

반응식

HRID 2099499 반응식
[NH:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)[NH2:2].Cl.[C:10]([O-])(O)=O.[Na+].[CH3:15][CH2:16]O>O.CCOC(C)=O>[N:1]1([C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=2)[CH:15]=[CH:16][CH:10]=[N:2]1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 786452-HydrazinopyridineHCID 516892Sodium Bicarbonate

생성물 1

HCID 53240862-(1H-pyrazol-1-yl)pyridine

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

2-Hydrazinopyridine (7.6 g, 70 mmol), malondialdehyde-bis-(dimethylacetal) (11.5 mL, 70 mmol) and HCl (10 M, 7 mL) in EtOH (100 mL) were heated at 75° C. After 2 h, the resulting reaction mixture was cooled to ambient temperature and concentrated in vacuo to a give a brown solid. This was suspended in H2O (100 mL) and EtOAc (100 mL), and NaHCO3 added until there was no further effervescence. The EtOAc layer was then separated and the aqueous layer shaken with EtOAc (3×100 mL). The combined organic layers were dried over Na2SO4 and concentrated to afford 2-(1H-pyrazol-1-yl)pyridine as a brown oil which was used without further purification. MS (ESI) 147 (M+H)+

후처리

  1. customthe resulting reaction mixture
  2. concentrationconcentrated in vacuo to
  3. customa give a brown solid
  4. customThe EtOAc layer was then separated
  5. dry with materialThe combined organic layers were dried over Na2SO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8398d2fefba545eb94c1ef32027f2a67
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07569592B2

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