Water → 2-(2-Phenyl-ethen-1-yl)-3-difluoromethoxy-thiophene-2-carboxanilide

HRID 1861823노트

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HRID 1861823 반응식
[C:1]1([CH:7]=[CH:8]C2C=CC=CC=2N)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([N:18]([CH2:21][CH3:22])CC)C.[F:23][CH:24]([F:34])[O:25][C:26]1[CH:30]=[CH:29][S:28][C:27]=1[C:31](Cl)=[O:32].O>C1(C)C=CC=CC=1>[C:1]1([CH:7]=[CH:8][C:27]2([C:31]([NH:18][C:21]3[CH:22]=[CH:3][CH:2]=[CH:1][CH:6]=3)=[O:32])[CH:26]([O:25][CH:24]([F:34])[F:23])[CH:30]=[CH:29][S:28]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 139378AminostilbeneHCID 111275992-Thiophenecarbonyl chloride, 3-(difluoromethoxy)-

생성물 1

HCID 698864132-(2-Phenyl-ethen-1-yl)-3-difluoromethoxy-thiophene-2-carboxanilide수율 189.2%

시약·촉매·용매 1

HCID 1140Toluene용매2회

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온도
50 °C

실험 절차

At room temperature, a solution of 0.3 g (0.0015 mol) of 2-(2-phenyl-ethen-1-yl)-aniline in 2 ml of toluene is admixed with a solution of 0.15 g (0.0015 mol) of triethylamine in 10 ml of toluene. At room temperature, 0.33 g (0.0015 mol) of 3-difluoromethoxy-thiophene-2-carbonyl chloride are added to this mixture with stirring. The mixture is subsequently heated to 50° C. and stirred at this temperature for 2 hours. For work-up, the reaction mixture is then cooled to room temperature and admixed with water. The organic phase is separated off, dried over sodium sulphate and then concentrated under reduced pressure at 60° C. The residue that remains is chromatographed over silica gel using diethyl ether. Concentration of the eluate gives 0.53 g (95% of theory) of 2-(2-phenyl-ethen-1-yl)-3-difluoromethoxy-thiophene-2-carboxanilide in the form of a solid substance of melting point 80 to 82° C.

후처리

  1. customAt room temperature
  2. stirringstirred at this temperature for 2 hours
  3. temperatureFor work-up, the reaction mixture is then cooled to room temperature
  4. customThe organic phase is separated off
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated under reduced pressure at 60° C
  7. customThe residue that remains is chromatographed over silica gel

출처 및 근거

ORD 기록
ord-c17673300eb143d481dd8e9539ba6298
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06534532B1

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