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

HRID 411826

반응식

HRID 411826 반응식
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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27773904-(Trifluoromethyl)benzenecarboximidamideHCID 18541697HCID 18541697, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-ab955588beac4678837f619742f8937b
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06559307B2

연결된 노트

불러오는 중…