反应详情

温度

65 °C

A suspension of 1-amino-2-[3-(3-formylphenoxy)propylamino]-1-cyclobutene-3,4-dione (6.0 g, 21.8 mmole) in 150 mL of toluene was treated with piperidine (4.3 mL, 3.7 g, 43.6 mmole) and the mixture was heated to 65° C., and then cooled to about 30° C. Formic acid (2.2 mL of 95% aqueous formic acid containing 2.5 g formic acid, 55.4 mmole) was added. The mixture was heated to reflux temperature and the water formed was collected by azeotropic distillation. When the distillate became clear and gas evolution had ceased (about 30 minutes at reflux), the mixture was cooled and the solids were collected by filtration, washed with toluene, methanol and dried to yield 4.7 g (62.8%) of the title compound; mp=223°-228° C.

1. temperaturecooled to about 30° C
2. temperatureThe mixture was heated
3. temperatureto reflux temperature
4. distillationwas collected by azeotropic distillation
5. temperature(about 30 minutes at reflux)
6. temperaturethe mixture was cooled
7. filtrationthe solids were collected by filtration
8. washwashed with toluene, methanol
9. customdried