反应详情

温度

20 °C

5 g (26.9 mmol) of N-(2-chloro-5-pyridylmethyl)ethylene-diamine and 11.7 g (84.6 mmol) of potassium carbonate are placed in 40 ml of methanol. A solution of 3.64 g (28.2 mmol) of 1,1,1-trifluoro-2-nitro-ethane in 20 ml of methanol is added dropwise at 5° C. to 10° C. within 30 minutes. After the addition is complete, the mixture is stirred for 5 hours at 20° C. The mixture is then concentrated by removal of the solvent by distillation in vacuo, and the residue is taken up in methylene chloride, washed with a small amount of water, dried, concentrated and recrystallized from methanol. 4.6 g (70.1% of theory) of 1-(2-chloro-5-pyridylmethyl)-2-(nitromethylene)-imidazoline of a melting point of 160° C. to 161° C. are obtained.

1. additionAfter the addition
2. concentrationThe mixture is then concentrated by removal of the solvent by distillation in vacuo
3. washwashed with a small amount of water
4. customdried
5. concentrationconcentrated
6. customrecrystallized from methanol