反应详情

A 500 ml., 3-neck, r.b. flask fitted with stirrer, condenser, and thermometer was charged with a mixture of the compound of Example I, C. (21.7 g., 0.1 mole), 3-chloro-4-methylaniline (14.2 g., 0.1 mole) and ethanol (300 ml.). The mixture was heated at reflux, while stirring, overnight. The near solution was concentrated to dryness by rotary evaporator and the residue was collected and dried to yield 35 g. (97.5%), m.p. 352°-364°C (dec). A 10 g. sample was dissolved in methanol (200 ml.), treated with charcoal and filtered while hot. Ether (ca 750 ml.) was added until the filtrate remained turbid and was then chilled. The crystals were collected by filtration and dried to yield 3.4 g. yellow crystals, m.p. 362°-370°C (dec). After two recrystallizations a m.p. 368°-372°C (dec) was obtained.

1. customflask fitted with stirrer, condenser
2. temperatureThe mixture was heated
3. temperatureat reflux
4. concentrationThe near solution was concentrated to dryness by rotary evaporator
5. customthe residue was collected
6. customdried
7. customto yield 35 g
8. filtrationfiltered while hot
9. additionEther (ca 750 ml.) was added until the filtrate
10. temperaturewas then chilled
11. filtrationThe crystals were collected by filtration
12. customdried
13. customto yield 3.4 g
14. customAfter two recrystallizations a m.p. 368°-372°C (dec)
15. customwas obtained