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Potassium Acetate → HCID 58355527、化合物

HRID 1184214
ノート
印刷プレビュー

反応式

HRID 1184214 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 517044Potassium AcetateHCID 58355151HCID 58355151、化合物

生成物 1

HCID 58355527HCID 58355527、化合物収率 47.5%

試薬・触媒・溶媒 2

HCID 178502593HCID 178502593、化合物触媒HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2832272bed5045fda8bb975caf2195f4
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08664380B2

反応ノート

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