Potassium Carbonate → Diethyl 1-[2-(2,4-dichlorophenyl)-2-oxoethyl]-1H-pyrazole-3,5-dicarboxylate

HRID 57669

反応式

HRID 57669 の反応式
[NH:1]1[C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[N:2]1.[CH:16]1[C:21]([Cl:22])=[CH:20][C:19]([Cl:23])=[C:18]([C:24]([CH2:26]Br)=[O:25])[CH:17]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:23][C:19]1[CH:20]=[C:21]([Cl:22])[CH:16]=[CH:17][C:18]=1[C:24](=[O:25])[CH2:26][N:1]1[C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[N:2]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 758282-Bromo-1-(2,4-dichlorophenyl)ethan-1-oneHCID 142184diethyl 1H-pyrazole-3,5-dicarboxylate

生成物 1

HCID 58169992Diethyl 1-[2-(2,4-dichlorophenyl)-2-oxoethyl]-1H-pyrazole-3,5-dicarboxylate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

5 g (23.6 mmol) of diethyl 1H-pyrazole-3,5-dicarboxylate were dissolved in 100 ml of acetone, and 6.3 g (23.6 mmol) of 2-bromo-2,4-dichloroacetophenone and 3.6 g (26 mmol) of potassium carbonate were added. The mixture was stirred at RT for 12 h. The reaction mixture was concentrated and the residue was taken up in water and dichloromethane. The organic phase was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated on a rotary evaporator. The residue was triturated with diethyl ether, and the solid was filtered off with suction. This gave 9.48 g (94% of theory) of the product as a solid.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. washThe organic phase was washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated on a rotary evaporator
  5. customThe residue was triturated with diethyl ether
  6. filtrationthe solid was filtered off with suction

出典と根拠

ORDレコード
ord-4b0855f0058e4b348a1a896657cb4178
出典データセット
uspto-grants-2016_09
特許番号
US09434731B2

関連ノート

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