Reaktionsgleichung
[C:1]([OH:11])(=[O:10])[CH2:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[N+:12]([O-])([OH:14])=[O:13].S(=O)(=O)(O)O>>[N+:12]([C:7]1[CH:6]=[CH:5][C:4]([CH2:3][CH2:2][C:1]([OH:11])=[O:10])=[CH:9][CH:8]=1)([O-:14])=[O:13]Komponenten
Versuchsvorschrift
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.
Aufarbeitung
- customIn a 2-liter, 3-necked, round-bottomed flask equipped with mechanical stirrer
- additionthermometer, and addition funnel
- temperaturewas warmed to 50°
- temperatureto maintain it in a liquid state
- additionTo the warm liquid was added slowly dropwise over a 4 hour period
- customThe reaction is very exothermic so that a water cooling bath
- additionwas added occasionally
- customat 50° C
- stirringThe very thick reaction mixture was stirred for an additional 2 hours
- filtrationThe solid was collected by filtration
- washwashed repeatedly with a total of 6 liters of water
- customAfter air drying
- customthe entire sample was recrystallized from 800 ml of acetone
- customgiving a first crop of 150.4 g mp. 162°-164° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-badfa30f59d148bfacee3610ffb2d8fe
- Quelldatensatz
- uspto-grants-1982_08
- Patentnummer
- US04343893
Verknüpfte Notizen
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