Reaktionsgleichung
[NH2:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[CH3:9].[C:10](=[O:15])([O:12][CH2:13][CH3:14])N.N.[CH2:17]([OH:19])[CH3:18].[CH2:20]([OH:22])C>>[CH2:13]([O:12][C:10]([NH:1][C:2]1[CH:7]=[C:6]([NH:8][C:20]([O:19][CH2:17][CH3:18])=[O:22])[CH:5]=[CH:4][C:3]=1[CH3:9])=[O:15])[CH3:14]Komponenten
Reaktionsbedingungen
- Temperatur
- 40 °C
Versuchsvorschrift
122 g (1 mol) of 2,4-Diaminotoluene and 1782 g (20 mol) of ethyl carbamate are heated to 200° C. in the presence of 320 g of ethanol, with stirring, in a 5-liter stirrer autoclave, and 1300 ml of an ammonia/ethanol mixture are distilled off per hour. The autoclave is adjusted to a pressure of from 6 to 10 bar by means of a control valve and the ethanol concentration is kept constant by pumping in fresh ethanol. After a reaction time of 5 hours, the autoclave is left to cool down, emptied, and the alcohol is distilled at 40° to 90° C./90 mbar. The distillation residue (1224 g) is taken up with 1200 g of water at 95° C. and intensively stirred. 260 g of 2,4-bis-(ethoxycarbonylamino)-toluene precipitate after cooling of the solution to 40° C. and are filtered off. The 2,4-bis-(ethoxycarbonylamino)-toluene is again taken up with 300 g of boiling water, and reprecipitated at 40° C. 170.4 g (64.1% of theoretical) of 2,4-bis-(ethoxycarbonylamino)-toluene are obtained after drying over night in a drying cupboard at 90° C./100 mbar.
Aufarbeitung
- distillationare distilled off per hour
- customThe autoclave is adjusted to a pressure of from 6 to 10 bar by means of a control valve
- concentrationthe ethanol concentration
- temperatureto cool down
- distillationthe alcohol is distilled at 40° to 90° C./90 mbar
- customis taken up with 1200 g of water at 95° C.
- filtrationare filtered off
- customreprecipitated at 40° C
Quellen und Nachweise
- ORD-Eintrag
- ord-e3c433cda3634a79a4ee6e617280c635
- Quelldatensatz
- uspto-grants-1995_03
- Patentnummer
- US05399736
Verknüpfte Notizen
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