Cesium carbonate → Diphenyl Ether

HRID 17744

反応式

HRID 17744 の反応式
Cl[C:2]1[CH:30]=[CH:29][C:5]([O:6][C:7]2[CH:12]=[CH:11][C:10](N3C=C(C4C=CC=CC=4O)N=C3CC(C)C)=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.C([O-])([O-])=O.[Cs+].[Cs+].S([O-])(=O)(=O)C>CN(C=O)C.O>[C:7]1([O:6][C:5]2[CH:4]=[CH:3][CH:2]=[CH:30][CH:29]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

参加物

6

反応物 3

HCID 10796Cesium carbonateHCID 85257MethanesulfonateHCID 66977442{1-[4-(4-Chloro-phenoxy)-phenyl]-2-isobutyl-1H-imidazol-4-yl}phenol

生成物 1

HCID 7583Diphenyl Ether

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

{1-[4-(4-Chloro-phenoxy)-phenyl]-2-isobutyl-1H-imidazol-4-yl}phenol (2 mmol) was added to a solution of Cs2CO3 (10 eq., 20 mmol) in anhydrous DMF (5 ml). This was followed by addition of the mesylate obtained above and the reaction mixture was heated to 90° C. for 2-3 h. The reaction mixture was then cooled to rt, diluted with cold water and the product was extracted with DCM. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo to give desired phenyl ether.

後処理

  1. customobtained above and the reaction mixture
  2. temperatureThe reaction mixture was then cooled to rt
  3. extractionthe product was extracted with DCM
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c369aedc1ee3451f8ccc6e154241d3d3
出典データセット
uspto-grants-2010_06
特許番号
US07737285B2

関連ノート

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