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

HRID 409721노트

반응식

HRID 409721 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-75431944cc5e4845872847b2cdb3c85f
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08759528B2

반응 노트

불러오는 중…