反应详情

温度

130 °C

A mixture of 2A (77.1 g), hydrazine hydrate (46.4 g) and KOH (590 g) in diethylene glycol (250 ml) is heated at 130° C. for 2 h, the excess of hydrazine hydrate is distilled off and the temperature is raised to 200° C. for 2 h. The cooled mixture is poured into 18% HCl, the product is extracted into ether twice and the combined ethereal extracts are washed with water and dried (MgSO4). The solvent is removed in vacuo and the residue is distilled (bp 145°-148° C. at 20 mm Hg) to yield a colourless liquid (58.1 g, 80%).

1. distillationthe excess of hydrazine hydrate is distilled off
2. temperaturethe temperature is raised to 200° C. for 2 h
3. additionThe cooled mixture is poured into 18% HCl
4. extractionthe product is extracted into ether twice
5. washthe combined ethereal extracts are washed with water
6. dry with materialdried (MgSO4)
7. customThe solvent is removed in vacuo
8. distillationthe residue is distilled (bp 145°-148° C. at 20 mm Hg)