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Potassium Carbonate → HCID 57486431, 화합물

HRID 2424304
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HRID 2424304 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]([C:11]1[C:12]([CH3:18])=[N:13][N:14]([CH3:17])[C:15]=1[OH:16])=[O:10].[Cl:19][C:20]1[CH:25]=[C:24](Cl)[N:23]=[N:22][C:21]=1[O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[CH3:34].C(=O)([O-])[O-].[K+].[K+]>>[Cl:19][C:20]1[CH:25]=[C:24]([O:16][C:15]2[N:14]([CH3:17])[N:13]=[C:12]([CH3:18])[C:11]=2[C:9]([C:3]2[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=2[Cl:1])=[O:10])[N:23]=[N:22][C:21]=1[O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[CH3:34]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 11430Potassium CarbonateHCID 23013971HCID 23013971, 화합물HCID 178434070HCID 178434070, 화합물

생성물 1

HCID 57486431HCID 57486431, 화합물수율 80.6%

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온도
130 °C

실험 절차

109 mg (0.382 mmol) of (2,4-dichlorophenyl)(5-hydroxy-1,3-dimethyl-1H-pyrazol-4-yl)methanone, 1.62 g (6.35 mmol) of 4,6-dichloro-3-(2-methylphenoxy)pyridazine obtained in Example 1 (2) and 107 mg (0.775 mmol) of potassium carbonate were mixed, and the mixture was stirred at 130° C. for 14 hours. The reaction mixture was cooled up to room temperature, and purified by silica gel column chromatography (hexane:ethyl acetate, gradient) to obtain 155 mg (0.308 mmol, Yield: 80.6%) of (5-{[5-chloro-6-(2-methylphenoxy)-3-pyridazinyl]oxy}-1,3-dimethyl-1H-pyrazol-4-yl) (2,4-dichlorophenyl)methanone.

후처리

  1. temperatureThe reaction mixture was cooled up to room temperature
  2. custompurified by silica gel column chromatography (hexane:ethyl acetate, gradient)

출처 및 근거

ORD 기록
ord-651efc833e374f738994985bad709041
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07964531B2

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