反应详情

温度

0 °C

15 g (76 mmol) of 6-(4-cyanophenyl)-2H-pyridazin-3-one, 22.2 g (114 mmol) of ethyl(3-hydroxymethylphenyl)carbamate and 29.9 g (114 mmol) of triphenylphosphine are dissolved in 250 ml of THF. Under a nitrogen atmosphere, the reaction mixture is cooled to 0° C., 18 ml (174 mmol) of diethyl azodicarboxylate are slowly added dropwise, and the reaction mixture is stirred at room temperature for 72 h. The reaction mixture is evaporated to dryness. 200 ml of isopropanol are added to the residue, and the mixture is stirred for 15 h. The precipitate is filtered off with suction, washed with isopropanol and dried in vacuo.

1. customThe reaction mixture is evaporated to dryness
2. addition200 ml of isopropanol are added to the residue
3. stirringthe mixture is stirred for 15 h
4. filtrationThe precipitate is filtered off with suction
5. washwashed with isopropanol
6. customdried in vacuo