反应详情

温度

0 °C

A solution of 30.2 g (0.20 mol) of 2-methoxy-6-fluorobenzonitrile [preparation: J. Heterocycl. Chem. 25 (1988), 1173]in 50 ml of N,N-dimethylformamide is added dropwise at 45°-50° C., under nitrogen, to a solution of 0.21 mol of sodium triazolide (prepared from equimolar amounts of triazol and sodium hydride) in 100 ml of N,N-dimethylformamide, and the mixture is stirred for 2 h at 0° C. After the solvent has been evaporated under reduced pressure, the residue is stirred with 200 ml of ice water, the pH is brought to 6 with a little glacial acetic acid and the solid is filtered off under suction and dried. After the addition of a little ether, 35 g of the product of melting point 169°-171° C. (decomposition) are obtained.

1. customAfter the solvent has been evaporated under reduced pressure
2. stirringthe residue is stirred with 200 ml of ice water
3. filtrationthe solid is filtered off under suction
4. customdried
5. additionAfter the addition of a little ether, 35 g of the product of melting point 169°-171° C. (decomposition)
6. customare obtained