Potassium Carbonate → HCID 58355158, 화합물

HRID 1259917노트

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HRID 1259917 반응식
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][N:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[C:16](Cl)(Cl)Cl.[CH3:20][CH:21]([CH3:37])[CH2:22][NH:23][C@H:24]1[CH2:29][CH2:28][CH2:27][N:26]([C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:25]1.C(=O)([O-])[O-:39].[K+].[K+]>C(#N)C.O.[Cl-].[Na+].O>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][N:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[C:16]([N:23]([CH2:22][CH:21]([CH3:37])[CH3:20])[C@H:24]1[CH2:29][CH2:28][CH2:27][N:26]([C:30]([O:32][C:33]([CH3:35])([CH3:34])[CH3:36])=[O:31])[CH2:25]1)=[O:39]

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 53256912HCID 53256912, 화합물HCID 67025978HCID 67025978, 화합물

생성물 1

HCID 58355158HCID 58355158, 화합물수율 62.7%

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 57417360Sodium chloride; water용매

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온도
80 °C

실험 절차

1-(4-Methoxybutyl)-2-(trichloromethyl)-1H-benzimidazole (470 mg) and tert-butyl (3S)-3-[(2-methylpropyl)amino]piperidine-1-carboxylate (400 mg) were dissolved in acetonitrile (30 ml) and water (15 ml), potassium carbonate (2.02 g) was added, and the mixture was stirred at 80° C. for 15 hr. The reaction mixture was cooled to room temperature and diluted with saturated brine. The mixture was extracted with ethyl acetate, and the extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate-hexane (60:40) was concentrated under reduced pressure to give the object product (446 mg).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. washthe extract was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. washa fraction eluted with ethyl acetate-hexane (60:40)
  7. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c14fb685fbc54af9a946139bc83b105a
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466282B2

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