2-(4-Chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-4-methyl-pentane-1,3-dione → HCID 68704522、化合物

HRID 14460ノート

反応式

HRID 14460 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:20](=[O:24])[CH:21]([CH3:23])[CH3:22])[C:9]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[C:13]([F:18])[C:12]=2O)=[O:10])=[CH:4][CH:3]=1>C(O)(=O)C.Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9](=[O:10])[C:11]3[C:12](=[C:13]([F:18])[C:14]([F:17])=[CH:15][CH:16]=3)[O:24][C:20]=2[CH:21]([CH3:23])[CH3:22])=[CH:6][CH:7]=1

参加物

4

反応物 1

HCID 686997002-(4-Chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-4-methyl-pentane-1,3-dione

生成物 1

HCID 68704522HCID 68704522、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒

反応条件

温度
140 °C

実験手順

A mixture of 2-(4-chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-4-methyl-pentane-1,3-dione (3.65 g, 10.3 mmol) in acetic acid (36 ml) and concentrated HCl solution (2 ml) is stirred at 140° C. for 3 h. The reaction mixture is cooled to room temperature, poured onto ice-water and extracted with methylene chloride. The organic layer is washed with saturated sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate and evaporated to dryness in vacuo to afford the title compound as a brown solid.

後処理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. additionpoured onto ice-water
  3. extractionextracted with methylene chloride
  4. washThe organic layer is washed with saturated sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-fa224b4cc0cd49ce92d0db54d17f8641
出典データセット
uspto-grants-2010_06
特許番号
US07732435B2

反応ノート

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