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Potassium Acetate → HCID 58355527, 화합물

HRID 1184214
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HRID 1184214 반응식
Cl[C:2]1[N:3]=[C:4]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[N:5]([CH2:35][CH2:36][CH2:37][CH2:38][O:39][CH3:40])[C:6]=1[C:7]([N:9]([CH2:31][CH:32]([CH3:34])[CH3:33])[C@H:10]1[CH2:15][C@@H:14]([C:16]([N:18]2[CH2:23][CH2:22][O:21][CH2:20][CH2:19]2)=[O:17])[CH2:13][N:12]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:11]1)=[O:8].C([O-])(=O)C.[K+]>CO.[OH-].[Pd+2].[OH-].[C]>[CH3:40][O:39][CH2:38][CH2:37][CH2:36][CH2:35][N:5]1[C:6]([C:7]([N:9]([CH2:31][CH:32]([CH3:33])[CH3:34])[C@H:10]2[CH2:15][C@@H:14]([C:16]([N:18]3[CH2:19][CH2:20][O:21][CH2:22][CH2:23]3)=[O:17])[CH2:13][N:12]([C:24]([O:26][C:27]([CH3:30])([CH3:28])[CH3:29])=[O:25])[CH2:11]2)=[O:8])=[CH:2][N:3]=[C:4]1[C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 517044Potassium AcetateHCID 58355151HCID 58355151, 화합물

생성물 1

HCID 58355527HCID 58355527, 화합물수율 47.5%

시약·촉매·용매 2

HCID 178502593HCID 178502593, 화합물촉매HCID 887Methanol용매

실험 절차

tert-Butyl(3S,5R)-3-[{[4-chloro-1-(4-methoxybutyl)-2-phenyl-1H-imidazol-5-yl]carbonyl}(2-methylpropyl)amino]-5-(morpholin-4-ylcarbonyl)piperidine-1-carboxylate (200 mg), palladium(II) hydroxide-carbon (20 mg) and potassium acetate (30 mg) were suspended in methanol (10 ml), and the mixture was stirred under a hydrogen atmosphere (1 atom) at room temperature for 1 day. The palladium catalyst was filtered off and the filtrate was concentrated under reduced pressure. The residue was suspended in water, and the suspension was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium 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 (10:90-80:20) was concentrated under reduced pressure to give the object product (90 mg).

후처리

  1. filtrationThe palladium catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. extractionthe suspension was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. washa fraction eluted with ethyl acetate-hexane (10:90-80:20)
  8. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2832272bed5045fda8bb975caf2195f4
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08664380B2

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