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Potassium Carbonate → (5-Chloro-2,6-dimethylpyrimidin-4-yl)[3-methoxy-4-(3-nitroimidazo[1,2-b]pyridazin-6-yloxy)benzyl]amine

HRID 2415093
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HRID 2415093 반응식
[Cl:1][C:2]1[C:3]([NH:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([OH:18])=[C:14]([O:19][CH3:20])[CH:13]=2)=[N:4][C:5]([CH3:9])=[N:6][C:7]=1[CH3:8].Cl[C:22]1[CH:23]=[CH:24][C:25]2[N:26]([C:28]([N+:31]([O-:33])=[O:32])=[CH:29][N:30]=2)[N:27]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Cl:1][C:2]1[C:3]([NH:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][C:22]3[CH:23]=[CH:24][C:25]4[N:26]([C:28]([N+:31]([O-:33])=[O:32])=[CH:29][N:30]=4)[N:27]=3)=[C:14]([O:19][CH3:20])[CH:13]=2)=[N:4][C:5]([CH3:9])=[N:6][C:7]=1[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 105359816-Chloro-3-nitro-imidazo(1,2-b)pyridazineHCID 226400084-[(5-Chloro-2,6-dimethylpyrimidin-4-ylamino)methyl]-2-methoxyphenol

생성물 1

HCID 22640011(5-Chloro-2,6-dimethylpyrimidin-4-yl)[3-methoxy-4-(3-nitroimidazo[1,2-b]pyridazin-6-yloxy)benzyl]amine

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

In analogy to the method described in example 1, 1.25 g (4.25 mmol) of 4-[(5-chloro-2,6-dimethyl-pyrimidin-4-ylamino)methyl]-2-methoxyphenol (from example B3), 0.86 g (4.25 mmol) of 6-chloro-3-nitroimidazo[1,2-b]pyridazine and 3.0 g (21.25 mmol) of potassium carbonate are reacted in 25 ml of dimethylformamide. After chromatography on silica gel (mobile phase: gradient toluene/dioxane 5:1 to 2:1) and crystallization from methylene chloride/methanol, 1.24 g (64%) of the title compound are isolated as a pale beige solid. m.p.: 229-232° C.

후처리

  1. customAfter chromatography on silica gel (mobile phase: gradient toluene/dioxane 5:1 to 2:1) and crystallization from methylene chloride/methanol, 1.24 g (64%) of the title compound
  2. customare isolated as a pale beige solid

출처 및 근거

ORD 기록
ord-9da2c7d858df409da1a49aefead8b7f6
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06818642B2

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