Ammonium formate → HCID 67059966, 화합물

HRID 238281노트

반응식

HRID 238281 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[CH2:11][CH2:12][N:13]([C:16](=[O:18])[CH3:17])[CH2:14][CH:15]=1)([O-])=O.C([O-])=O.[NH4+]>O.[Pd]>[NH2:1][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH:10]1[CH2:11][CH2:12][N:13]([C:16](=[O:18])[CH3:17])[CH2:14][CH2:15]1

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 68008288HCID 68008288, 화합물

생성물 1

HCID 67059966HCID 67059966, 화합물수율 76.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

실험 절차

1-[4-(2-Nitro-phenyl)-3,6-dihydro-2H-pyridin-1-yl]ethanone (0.43 g, 1.8 mmol) was dissolved in a solution of ammonium formate (1.13 g, 18 mmol) in IMS (20 mL) and water (20 mL). Palladium on carbon (10% w/w, 0.2 g) was then added and the mixture heated at reflux for 1 hour. The solution was filtered and then the solvent removed by evaporation under vacuum. The residue was dissolved in ethyl acetate (50 mL) and the resulting solution washed with saturated aqueous sodium hydrogen carbonate solution, dried over magnesium sulphate, filtered and the solvent removed by evaporation under vacuum to give the title compound as a pale pink oil (0.3 g). LCMS m/z 219.38 [M+H]+. R.T.=2.29 min (Analytical Method 4).

후처리

  1. temperaturethe mixture heated
  2. temperatureat reflux for 1 hour
  3. filtrationThe solution was filtered
  4. customthe solvent removed by evaporation under vacuum
  5. dissolutionThe residue was dissolved in ethyl acetate (50 mL)
  6. washthe resulting solution washed with saturated aqueous sodium hydrogen carbonate solution
  7. dry with materialdried over magnesium sulphate
  8. filtrationfiltered
  9. customthe solvent removed by evaporation under vacuum

출처 및 근거

ORD 기록
ord-ed742dd693e74b56850b79ff6a6c8994
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642621B2

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