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1,1'-Carbonyldiimidazole → 1-[5-tert-butyl-2-(4-nitrophenyl)-2H-pyrazol-3-yl]-3-[4-(pyridin-4-yloxy)phenyl]urea

HRID 221883
ノート
印刷プレビュー

反応式

HRID 221883 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([NH2:19])[N:8]([C:10]2[CH:15]=[CH:14][C:13]([N+:16]([O-:18])=[O:17])=[CH:12][CH:11]=2)[N:9]=1)([CH3:4])([CH3:3])[CH3:2].C1N=CN([C:25]([N:27]2C=N[CH:29]=[CH:28]2)=[O:26])C=1.[N:32]1[CH:37]=[CH:36][C:35]([O:38][C:39]2[CH:44]=CC(N)=[CH:41][CH:40]=2)=[CH:34][CH:33]=1>ClCCCl>[C:1]([C:5]1[CH:6]=[C:7]([NH:19][C:25]([NH:27][C:28]2[CH:29]=[CH:44][C:39]([O:38][C:35]3[CH:36]=[CH:37][N:32]=[CH:33][CH:34]=3)=[CH:40][CH:41]=2)=[O:26])[N:8]([C:10]2[CH:15]=[CH:14][C:13]([N+:16]([O-:18])=[O:17])=[CH:12][CH:11]=2)[N:9]=1)([CH3:4])([CH3:2])[CH3:3]
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 3

HCID 682631,1'-CarbonyldiimidazoleHCID 13023603-tert-butyl-1-(4-nitrophenyl)-1H-pyrazol-5-amineHCID 115645894-(Pyridin-4-yloxy)aniline

生成物 1

HCID 536301901-[5-tert-butyl-2-(4-nitrophenyl)-2H-pyrazol-3-yl]-3-[4-(pyridin-4-yloxy)phenyl]urea収率 68%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒2 回

実験手順

To a solution of 5-tert-butyl-2-(4-nitrophenyl)-2H-pyrazol-3-ylamine (5.0 g, 19.2 mmol) in anhydrous DCE (2 mL) was added CDI (3.5 g, 21.1 mmol), and the reaction was stirred under N2 at room temperature for 18 h. 4-(Pyridin-4-yloxy)phenylamine (3.3 g, 17.7 mmol, Dumas et al., U.S. pat. appl. US2002065296 (2002)) in DCE (12 mL) was added to the reaction, and the solution was stirred under N2 at room temperature for 7 h. The reaction mixture was partitioned between EtOAc (100 mL) and water (100 mL). The organic layer was washed with brine, dried over Na2SO4, and concentrated at reduced pressure. The crude residue was purified by MPLC (1:1 hexanes/EtOAc) to give 5.6 g (68%) of the desired product. 1H-NMR (DMSO-d6) δ 9.21 (s, 1H), 8.68 (s, 1H), 8.43 (d, J=6.3 Hz, 2H), 8.36 (d, J=7.2 Hz, 2H), 7.90 (d, J=6.9 Hz, 2H), 7.50 (d, J=6.9 Hz, 2H), 7.09 (d, J=6.6 Hz, 2H), 6.86 (d, J=5.7 Hz, 2H), 6.44 (s, 1H), 1.29 (s, 9H); MS LC-MS [M+H]+=473, RT=2.60 min.

後処理

  1. stirringthe solution was stirred under N2 at room temperature for 7 h
  2. customThe reaction mixture was partitioned between EtOAc (100 mL) and water (100 mL)
  3. washThe organic layer was washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated at reduced pressure
  6. customThe crude residue was purified by MPLC (1:1 hexanes/EtOAc)

出典と根拠

ORDレコード
ord-393465ebc2b14ab0bd77b3d95829f2f9
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08207166B2

反応ノート

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