反应详情

温度

60 °C

A solution of 0.273 mol of sodium pyrazolide (prepared from equimolar amounts of pyrazole and sodium hydride) in 140 ml of N,N-dimethylethyleneurea is added dropwise at 50° C., under nitrogen, to a solution of 41.2 g (0.273 mol) of 2-methoxy-6-fluorobenzonitrile (preparation: J. Heterocycl. Chem. 25 (1988), 1173) in 50 ml N,N-dimethylethyleneurea and the mixture is stirred at 60° C. for 2h. After the mixture has been cooled and stirred into 4 l of ice water and the precipitated crystals have been filtered off under suction and dried, 37.1 g of the product of melting point 93°-94° C. are obtained.

1. temperatureAfter the mixture has been cooled
2. filtrationthe precipitated crystals have been filtered off under suction
3. customdried