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Water → HCID 58046321、化合物

HRID 2359332
ノート
印刷プレビュー

反応式

HRID 2359332 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 58046321HCID 58046321、化合物収率 75.5%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide
溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-dadcef30da80419ba55cab29f243f700
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08685977B2

反応ノート

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