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Potassium Carbonate → N-(4-((2-Aminopyridin-4-yl)oxy)-2,5-difluorophenyl)-4-ethoxy-1-(4-fluorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide

HRID 1411156
ノート
印刷プレビュー

反応式

HRID 1411156 の反応式
C([NH:4][C:5]1[CH:10]=[C:9]([O:11][C:12]2[C:17]([F:18])=[CH:16][C:15]([NH:19][C:20]([C:22]3[C:23](=[O:38])[N:24]([C:31]4[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=4)[CH:25]=[CH:26][C:27]=3[O:28][CH2:29][CH3:30])=[O:21])=[C:14]([F:39])[CH:13]=2)[CH:8]=[CH:7][N:6]=1)(=O)C.C([O-])([O-])=O.[K+].[K+]>CCO>[NH2:4][C:5]1[CH:10]=[C:9]([O:11][C:12]2[C:17]([F:18])=[CH:16][C:15]([NH:19][C:20]([C:22]3[C:23](=[O:38])[N:24]([C:31]4[CH:32]=[CH:33][C:34]([F:37])=[CH:35][CH:36]=4)[CH:25]=[CH:26][C:27]=3[O:28][CH2:29][CH3:30])=[O:21])=[C:14]([F:39])[CH:13]=2)[CH:8]=[CH:7][N:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 71566461N-(4-((2-acetamidopyridin-4-yl)oxy)-2,5-difluorophenyl)-4-ethoxy-1-(4-fluorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide

生成物 1

HCID 68252797N-(4-((2-Aminopyridin-4-yl)oxy)-2,5-difluorophenyl)-4-ethoxy-1-(4-fluorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide収率 38%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of Example 1 (1.00 g, 1.86 mmol) and K2CO3 (1.000 g, 7.24 mmol) in EtOH (4 mL) was heated at 120° C. under microwave irradiation for 1 h. The reaction mixture was filtered, washed with EtOH and the filtrate was evaporated to dryness. The crude was stirred in water (15 mL) for a few minutes and collected by filtration. The residue was further purified by successive crystallization from MeOH and MeCN to provide N-(4-((2-aminopyridin-4-yl)oxy)-2,5-difluorophenyl)-4-ethoxy-1-(4-fluorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide (350 mg, 38.0% yield) as a white solid. MS (ESI) m/z: 497.1 (M+H+).

後処理

  1. filtrationThe reaction mixture was filtered
  2. washwashed with EtOH
  3. customthe filtrate was evaporated to dryness
  4. filtrationcollected by filtration
  5. customThe residue was further purified by successive crystallization from MeOH and MeCN

出典と根拠

ORDレコード
ord-609f8bf7506e46ee81391511ae4bc3cc
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08921565B2

反応ノート

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