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

HRID 14460노트

반응식

HRID 14460 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

HCID 68704522HCID 68704522, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매

반응 조건

온도
140 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fa224b4cc0cd49ce92d0db54d17f8641
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732435B2

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