反应详情

In a 2-liter, 3-necked, round-bottomed flask equipped with mechanical stirrer, thermometer, and addition funnel was placed 361 g (2.41 mol) of hydrocinnamic acid which was warmed to 50° to maintain it in a liquid state. To the warm liquid was added slowly dropwise over a 4 hour period with good stirring a mixture of 241 g of nitric acid and 546 g of sulfuric acid. The reaction is very exothermic so that a water cooling bath was required to which ice was added occasionally to keep the temperature at 50° C. The very thick reaction mixture was stirred for an additional 2 hours and poured onto 3 liters of ice. The solid was collected by filtration and washed repeatedly with a total of 6 liters of water. After air drying, the entire sample was recrystallized from 800 ml of acetone, giving a first crop of 150.4 g mp. 162°-164° C.

1. customIn a 2-liter, 3-necked, round-bottomed flask equipped with mechanical stirrer
2. additionthermometer, and addition funnel
3. temperaturewas warmed to 50°
4. temperatureto maintain it in a liquid state
5. additionTo the warm liquid was added slowly dropwise over a 4 hour period
6. customThe reaction is very exothermic so that a water cooling bath
7. additionwas added occasionally
8. customat 50° C
9. stirringThe very thick reaction mixture was stirred for an additional 2 hours
10. filtrationThe solid was collected by filtration
11. washwashed repeatedly with a total of 6 liters of water
12. customAfter air drying
13. customthe entire sample was recrystallized from 800 ml of acetone
14. customgiving a first crop of 150.4 g mp. 162°-164° C.