Triethylamine → 3-Methyl 1-(4-nitrophenyl) 5-(4-ethylphenyl)piperidine-1,3-dicarboxylate

HRID 876260노트

반응식

HRID 876260 반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:14][NH:13][CH2:12][CH:11]([C:15]([O:17][CH3:18])=[O:16])[CH2:10]2)=[CH:5][CH:4]=1)[CH3:2].C(N(CC)CC)C.Cl[C:27]([O:29][C:30]1[CH:35]=[CH:34][C:33]([N+:36]([O-:38])=[O:37])=[CH:32][CH:31]=1)=[O:28]>ClCCl>[CH2:1]([C:3]1[CH:4]=[CH:5][C:6]([CH:9]2[CH2:14][N:13]([C:27]([O:29][C:30]3[CH:31]=[CH:32][C:33]([N+:36]([O-:38])=[O:37])=[CH:34][CH:35]=3)=[O:28])[CH2:12][CH:11]([C:15]([O:17][CH3:18])=[O:16])[CH2:10]2)=[CH:7][CH:8]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 821294-Nitrophenyl chloroformateHCID 58002552Methyl 5-(4-ethylphenyl)piperidine-3-carboxylate

생성물 1

HCID 580023823-Methyl 1-(4-nitrophenyl) 5-(4-ethylphenyl)piperidine-1,3-dicarboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

10.0 g (40.4 mmol) of the compound from Example 2A were initially charged in 135 ml of dichloromethane and cooled to 0° C., and 11.2 ml (8.2 g, 80.9 mmol) of triethylamine and 8.5 g (40.4 mmol) of 4-nitrophenyl chloroformate were added. The reaction mixture was allowed to warm to room temperature over a period of 2 h. For work-up, the mixture was twice washed with water, and the organic phase was dried over sodium sulphate. The solvent was removed under reduced pressure and the residue was dried under high vacuum. Yield: 16.5 g (83% of theory)

후처리

  1. temperatureto warm to room temperature over a period of 2 h
  2. washFor work-up, the mixture was twice washed with water
  3. dry with materialthe organic phase was dried over sodium sulphate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was dried under high vacuum

출처 및 근거

ORD 기록
ord-ba9f81bdab7b4713bc97c6141fd0f975
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987248B2

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