Ammonium formate → HCID 67059966、化合物

HRID 238281ノート

反応式

HRID 238281 の反応式
[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

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 68008288HCID 68008288、化合物

生成物 1

HCID 67059966HCID 67059966、化合物収率 76.3%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ed742dd693e74b56850b79ff6a6c8994
出典データセット
uspto-grants-2014_02
特許番号
US08642621B2

反応ノート

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