Water → N4-(4-methoxy-phenyl)-5-nitro-N2-(1-phenyl-1H-pyrazol-4-yl)-pyrimidine-2,4-diamine

HRID 1481246ノート

反応式

HRID 1481246 の反応式
C(N(C(C)C)CC)(C)C.Cl[C:11]1[N:16]=[C:15]([NH:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)[C:14]([N+:26]([O-:28])=[O:27])=[CH:13][N:12]=1.[C:29]1([N:35]2[CH:39]=[C:38]([NH2:40])[CH:37]=[N:36]2)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.O>O1CCOCC1>[CH3:25][O:24][C:21]1[CH:22]=[CH:23][C:18]([NH:17][C:15]2[C:14]([N+:26]([O-:28])=[O:27])=[CH:13][N:12]=[C:11]([NH:40][C:38]3[CH:37]=[N:36][N:35]([C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)[CH:39]=3)[N:16]=2)=[CH:19][CH:20]=1

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 1210211-Phenyl-1H-pyrazol-4-amineHCID 89717635(2-Chloro-5-nitro-pyrimidin-4-yl)-(4-methoxy-phenyl)-amine

生成物 1

HCID 89720564N4-(4-methoxy-phenyl)-5-nitro-N2-(1-phenyl-1H-pyrazol-4-yl)-pyrimidine-2,4-diamine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

284 g (19.0 mmol) Diisopropylethylamine are added to a solution of 561 mg (2.00 mmol) (2-chloro-5-nitro-pyrimidin-4-yl)-(4-methoxy-phenyl)-amine and 350 mg (2.00 mmol) 1-phenyl-1H-pyrazol-4-ylamine in 6 ml dioxane. The mixture is stirred for 16 hours at room temperature. Then water is added to the reaction mixture, the resulting precipitate is filtered off, washed with water and dried under vacuum giving N4-(4-methoxy-phenyl)-5-nitro-N2-(1-phenyl-1H-pyrazol-4-yl)-pyrimidine-2,4-diamine as yellow crystals; HPLC/MS (B): 2.50 min, [M+H] 404.

後処理

  1. filtrationthe resulting precipitate is filtered off
  2. washwashed with water
  3. customdried under vacuum

出典と根拠

ORDレコード
ord-f6427ea721d84cc7a99dcba602d8c388
出典データセット
uspto-grants-2016_08
特許番号
US09409914B2

反応ノート

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