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

HRID 1481246노트

반응식

HRID 1481246 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f6427ea721d84cc7a99dcba602d8c388
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409914B2

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