Potassium Carbonate → 4-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-Pyrimidine

HRID 411826

反応式

HRID 411826 の反応式
FC(F)(F)C1C=C(C=CC=1)O[C:7]([O:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=1)=[CH:8][CH:9]=O.[F:27][C:28]([F:39])([F:38])[C:29]1[CH:37]=[CH:36][C:32]([C:33]([NH2:35])=[NH:34])=[CH:31][CH:30]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[F:21][C:18]([F:19])([F:20])[C:14]1[CH:13]=[C:12]([CH:17]=[CH:16][CH:15]=1)[O:11][C:7]1[CH:8]=[CH:9][N:35]=[C:33]([C:32]2[CH:31]=[CH:30][C:29]([C:28]([F:27])([F:38])[F:39])=[CH:37][CH:36]=2)[N:34]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 27773904-(Trifluoromethyl)benzenecarboximidamideHCID 18541697HCID 18541697、化合物

生成物 1

HCID 99299504-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-Pyrimidine収率 80%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

A mixture of 3,3-bis-(3-trifluoromethylphenoxy)-acrolein (10 mmoles), 4-trifluoromethylbenzamidine (10 mmoles), potassium carbonate (10 mmoles) and acetonitril (100 ml), is stirred at 80° C. for four hours. The reaction mixture is cooled down to ambient temperature and filtered through silica. The organic phase is washed with ethyl acetate and concentrated in vacuo. The residue is purified by chromatography on Al2O3 (petrol ethers/ethyl acetate: 2/1) to yield 3.06 g (80%) of the pure product having a melting point of 66° C.

後処理

  1. temperatureThe reaction mixture is cooled down to ambient temperature
  2. filtrationfiltered through silica
  3. washThe organic phase is washed with ethyl acetate
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by chromatography on Al2O3 (petrol ethers/ethyl acetate: 2/1)

出典と根拠

ORDレコード
ord-ab955588beac4678837f619742f8937b
出典データセット
uspto-grants-2003_05
特許番号
US06559307B2

関連ノート

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