Potassium Carbonate → HCID 66926125、化合物
反応式
CO[C:3](=[O:22])[CH2:4][CH2:5][C:6](=[O:21])[CH2:7][N:8]1[C:12]([CH3:13])=[CH:11][C:10]([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)=[N:9]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Cl:20][C:17]1[CH:16]=[CH:15][C:14]([C:10]2[CH:11]=[C:12]([CH3:13])[N:8]([CH:7]3[C:3](=[O:22])[CH2:4][CH2:5][C:6]3=[O:21])[N:9]=2)=[CH:19][CH:18]=1参加物
4
反応条件
- 温度
- 200 °C
実験手順
5-[3-(4-chloro-phenyl)-5-methyl-pyrazol-1-yl]-4-oxo-pentanoic acid methyl ester (1.7 g, 5.5 mmol) was dissolved in dimethylformamide (16 ml) and anhydrous potassium carbonate (3 g, 22 mmol) added. The mixture was then heated to 200° C. for 10 mins in the microwave (using “normal” absorbtion). The reaction was reduced in vacuo, and partitioned between 2 M hydrochloric acid (50 ml) and dichloromethane (100 ml). The layers were separated, and the aqueous layer saturated with sodium chloride and extracted with dichloromethane (100 ml). The organics were combined, dried over magnesium sulfate and the solvent removed in vacuo. The reaction was then purified by column chromatography (using DCM:EtOAc:AcOH (9:1:0.01%) to (3:7:0.01%)) to give 2-[3-(4-chloro-phenyl)-5-methyl-pyrazol-1-yl]-cyclopentane-1,3-dione (0.8 g).