Diethyl Ether → Ethyl 1-benzoylpiperidine-4-carboxylate

HRID 962729노트

반응식

HRID 962729 반응식
[NH:1]1[CH2:11][CH2:10][CH:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH2:3][CH2:2]1.CCOCC.C(=O)([O-])[O-].[Na+].[Na+].[C:23](Cl)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C(OCC)(=O)C.O>[C:23]([N:1]1[CH2:2][CH2:3][CH:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH2:10][CH2:11]1)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 7412Benzoyl chlorideHCID 10340Sodium CarbonateHCID 70770Ethyl 4-piperidinecarboxylate

생성물 1

HCID 735824Ethyl 1-benzoylpiperidine-4-carboxylate수율 92%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a ice cold, stirred mixture of 55 g of ethyl isonipecotate, 200 mL of ether, 200 mL of saturated sodium carbonate and 200 mL of water was added dropwise 40 mL of benzoyl chloride. The resulting mixture was allowed to warm and stir overnight, diluted with 200 mL of ethyl acetate and separated. The organic layer was washed with 200 mL of 1N hydrochloric acid, dried over MgSO4, and concentrated. Drying the residue under vacuum gave 83.3 g (92%) of ethyl 1-benzoyl-4-piperidinecarboxylate as a white solid.

후처리

  1. temperatureto warm
  2. customseparated
  3. washThe organic layer was washed with 200 mL of 1N hydrochloric acid
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customDrying the residue under vacuum

출처 및 근거

ORD 기록
ord-d65b9e2e83804b12b1091a73126a5e22
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05760054

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