反应详情

温度

5 °C

A 500 ml. 3-neck, r.b. flask fitted with y-tube and condenser and thermometer, stirrer and addition funnel was charged with a mixture of 2-chloro-5-nitropyridine (15.8 g. 0.1 mole) in ethanol (300 ml.). To this was added N-methylpiperazine (20 g. 0.2 mole) dropwise while stirring. After the addition (ca. 5 min.), the mixture was heated at reflux for 3 hr. while stirring continued. The solution was chilled to 5°C and the crystals were collected by filtration and dried at 60°C to yield 12 g. yellow crystals, m.p. 94°-96°C.

1. customflask fitted with y-tube and condenser and thermometer, stirrer and addition funnel
2. additionAfter the addition (ca. 5 min.)
3. temperaturethe mixture was heated
4. temperatureat reflux for 3 hr
5. stirringwhile stirring
6. filtrationthe crystals were collected by filtration
7. customdried at 60°C
8. customto yield 12 g