Hydrochloric Acid → N-Ethyl-2-(4-piperidin-4-yl-phenyl)-propionamide

HRID 409721ノート

反応式

HRID 409721 の反応式
Cl.[CH2:2]([NH:4][C:5](=[O:20])[CH:6]([C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=2)=[CH:10][CH:9]=1)[CH3:7])[CH3:3]>C(O)C.[Pt](=O)=O>[CH2:2]([NH:4][C:5](=[O:20])[CH:6]([C:8]1[CH:13]=[CH:12][C:11]([CH:14]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)=[CH:10][CH:9]=1)[CH3:7])[CH3:3]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 86686108N-Ethyl-2-(4-pyridin-4-yl-phenyl)-propionamide

生成物 1

HCID 86686109N-Ethyl-2-(4-piperidin-4-yl-phenyl)-propionamide

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 702Ethanol溶媒

実験手順

4.4 mL 1N HCl are added to 1.12 g (4.40 mmol) N-ethyl-2-(4-pyridin-4-yl-phenyl)-propionamide (V.1) in 15 mL ethanol. The mixture is hydrogenated (5 bar) for 6 h at rt using 110 mg platinum(IV) oxide. After that time, the catalyst is filtered off and the solvent is evaporated. The residue is taken up in water, alkalized with 1N NaOH and extracted with DCM (2×). The organic layer is dried over magnesium sulphate and the solvent is evaporated. The residue is purified by HPLC (column: Gemini; eluent A: water+0.1% NH4OH, eluent B: MeOH) to yield the desired product.

後処理

  1. customfor 6 h
  2. customat rt
  3. filtrationAfter that time, the catalyst is filtered off
  4. customthe solvent is evaporated
  5. extractionextracted with DCM (2×)
  6. dry with materialThe organic layer is dried over magnesium sulphate
  7. customthe solvent is evaporated
  8. customThe residue is purified by HPLC (column: Gemini; eluent A: water+0.1% NH4OH, eluent B: MeOH)

出典と根拠

ORDレコード
ord-75431944cc5e4845872847b2cdb3c85f
出典データセット
uspto-grants-2014_06
特許番号
US08759528B2

反応ノート

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