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Potassium Carbonate → 2-(2,6-Difluorophenyl)-5-(4'-trifluoromethoxybiphenyl-4-yl)-pyrimidine

HRID 2119786
노트
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반응식

HRID 2119786 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[N:10][C:11]([C:14]3[C:19]([F:20])=[CH:18][CH:17]=[CH:16][C:15]=3[F:21])=[N:12][CH:13]=2)=[CH:4][CH:3]=1.[F:22][C:23]([F:36])([F:35])[O:24][C:25]1[CH:30]=[CH:29][C:28](OB(O)O)=[CH:27][CH:26]=1.C(=O)([O-])[O-].[K+].[K+]>C(COC)OC.O.CC(O)=O.CC(O)=O.[Pd]>[F:21][C:15]1[CH:16]=[CH:17][CH:18]=[C:19]([F:20])[C:14]=1[C:11]1[N:10]=[CH:9][C:8]([C:5]2[CH:6]=[CH:7][C:2]([C:28]3[CH:27]=[CH:26][C:25]([O:24][C:23]([F:22])([F:35])[F:36])=[CH:30][CH:29]=3)=[CH:3][CH:4]=2)=[CH:13][N:12]=1
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참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 227270174-Trifluoromethoxyphenylboric acidHCID 234433995-(4-Bromophenyl)-2-(2,6-difluorophenyl)-pyrimidine

생성물 1

HCID 114077102-(2,6-Difluorophenyl)-5-(4'-trifluoromethoxybiphenyl-4-yl)-pyrimidine

시약·촉매·용매 3

HCID 4144353Palladium (II) acetate촉매
HCID 962
Water
용매
HCID 80711,2-Dimethoxyethane용매

실험 절차

0.70 g of 5-(4-bromophenyl)-2-(2,6-difluorophenyl)-pyrimidine, 0.53 g of 4-trifluoromethoxyphenyl-boric acid and 0.07 g of palladium-II-acetate are heated under reflux for 1½ hours, under nitrogen, in a mixture of 20 ml of dimethoxyethane and 20 ml of saturated, aqueous potassium carbonate solution. The reaction mixture is then cooled, diluted with water and the crystalline precipitate filtered. After dissolving the precipitate in ethyl acetate, drying with magnesium sulfate, filtering and concentrating, the title compound is obtained in the form of light yellow crystals with a melting point of 215-216° C.

후처리

  1. temperatureThe reaction mixture is then cooled
  2. filtrationthe crystalline precipitate filtered
  3. dissolutionAfter dissolving the precipitate in ethyl acetate
  4. dry with materialdrying with magnesium sulfate
  5. filtrationfiltering
  6. concentrationconcentrating

출처 및 근거

ORD 기록
ord-7250a6f371b7471ab478931cd22d12ef
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06686469B2

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