甲基 2-(2-氟苯基)-2-氧代乙酸乙酯

反应条件: temp:22.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A suspension of 3.75 g of 80% pure NaH in 50 ml of dimethyl sulfoxide (DMSO) was admixed with 21.7 g of 3-bromo-4-fluorophenol (cf. DE-A 192 80 27) and then stirred at 20-25° C. for 30 min, and a solution of 22.7 g of methyl 2-(2-fluorophenyl)oxoacetate in 100 ml of DMSO was added dropwise. The reaction mixture was stirred at 20-25° C. for approximately 12 hours, poured into ice-water and then extracted with ethyl acetate. The organic phases were washed with 1 N aqueous sodium hydroxide solution and water and dried, and the solvent was distilled off, giving 35 g of the title compound. The reaction mixture was stirred at 20-25° C. for approximately 12 hours extracted with ethyl acetate The organic phases were washed with 1 N aqueous sodium hydroxide solution and water dried the solvent was distilled off

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 4.2 g of methyl 2-fluorophenylglyoxalate in 30 ml of anhydrous dimethyl sulfoxide was added dropwise to a solution of 5.0 g of the potassium salt of 1-(4-chlorophenyl)-3-hydroxy-pyrazole in 30 ml of anhydrous dimethyl sulfoxide. The batch was heated at 60° C. for 3.5 more hours, cooled and divided into two halves. One half was poured into ice-water/methyl tert-butyl ether for working-up. After the organic phase had been separated off, the aqueous phase was extracted three more times with methyl tert-butyl ether. The combined organic phases were dried over sodium sulfate and concentrated. The crude product was purified by chromatography over silica gel (eluent heptane/ethyl acetate 80/20→70/30). This gave 1.0 g of the title compound as a pale oil. cooled After the organic phase had been separated off the aqueous phase was extracted three more times with methyl tert-butyl ether The combined organic phases were dried over sodium sulfate concentrated The crude product was purified by chromatography over silica gel (eluent heptane/ethyl acetate 80/20→70/30)

反应条件: temp:22.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A suspension of 3.75 g of 80% pure NaH in 50 ml of dimethyl sulfoxide (DMSO) was admixed with 21.7 g of 3-bromo-4-fluorophenol (cf. DE-A 192 80 27) and then stirred at 20-25° C. for 30 min, and a solution of 22.7 g of methyl 2-(2-fluorophenyl)oxoacetate in 100 ml of DMSO was added dropwise. The reaction mixture was stirred at 20-25° C. for approximately 12 hours, poured into ice-water and then extracted with ethyl acetate. The organic phases were washed with 1 N aqueous sodium hydroxide solution and water and dried, and the solvent was distilled off, giving 35 g of the title compound. The reaction mixture was stirred at 20-25° C. for approximately 12 hours extracted with ethyl acetate The organic phases were washed with 1 N aqueous sodium hydroxide solution and water dried the solvent was distilled off