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Water → HCID 58046321, 화합물

HRID 2359332
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HRID 2359332 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([OH:13])[CH:5]=[CH:6][C:7]=1[O:8][C:9]([F:12])([F:11])[F:10].[Cl:14][C:15]1[C:16](F)=[CH:17][C:18]([F:28])=[C:19]([CH:27]=1)[C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21].C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[Cl:14][C:15]1[C:16]([O:13][C:4]2[CH:5]=[CH:6][C:7]([O:8][C:9]([F:11])([F:12])[F:10])=[C:2]([Cl:1])[CH:3]=2)=[CH:17][C:18]([F:28])=[C:19]([CH:27]=1)[C:20]([O:22][C:23]([CH3:24])([CH3:25])[CH3:26])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 404271083-Chloro-4-(trifluoromethoxy)phenolHCID 58042499Tert-butyl 5-chloro-2,4-difluorobenzoate

생성물 1

HCID 58046321HCID 58046321, 화합물수율 75.5%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide
용매

실험 절차

3-chloro-4-(trifluoromethoxy)phenol (22.6 g, 0.106 mol) and tert-butyl 5-chloro-2,4-difluorobenzoate (Preparation 51, 26.4 g, 0.106 mol) were dissolved in dimethlysulfoxide (105 mL). Then potassium carbonate (29.4 g, 0.213 mol) was added portionwise to the mixture, which was stirred at room temperature for 18 hours. The reaction mixture was dropped into iced water (500 mL) and stirred vigorously for 4 hours. The resulting solid was collected by filtration then taken up in isopropanol (75 mL) and water (15 mL). The reaction was heated to 55° C., then cooled down to room temperature. The resulting solid was collected by filtration to yield the title compound as an off-white white solid (35.3 g, 75%).

후처리

  1. stirringstirred vigorously for 4 hours
  2. filtrationThe resulting solid was collected by filtration
  3. temperatureThe reaction was heated to 55° C.
  4. temperaturecooled down to room temperature
  5. filtrationThe resulting solid was collected by filtration

출처 및 근거

ORD 기록
ord-dadcef30da80419ba55cab29f243f700
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08685977B2

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