Reaktionsgleichung
[C:1](Cl)(Cl)=[O:2].[C:5]([NH:15][NH2:16])(=[O:14])[CH2:6][CH2:7][CH2:8][CH2:9][C:10]([NH:12][NH2:13])=[O:11].[C:17]1([OH:23])C=CC=CC=1>>[O:11]1[C:17](=[O:23])[NH:13][N:12]=[C:10]1[CH2:9][CH2:8][CH2:7][CH2:6][C:5]1[O:14][C:1](=[O:2])[NH:16][N:15]=1Komponenten
Reaktionsbedingungen
- Temperatur
- 85 °C
Versuchsvorschrift
A solution of 200 g of phosgene in 1.6 kg of phenol was introduced at 20° C. into a 4-liter phosgenation apparatus, and 174 g of adipic acid dihydrazide were added thereto. The mixture was heated to 85° C. within one hour, with stirring; gas evolved above a reaction temperature of 45° C. Phosgene was then introduced into the reaction mixture at 85° C. over 5 hours (approx. 30 g per hour), with stirring. The solution was then purged with nitrogen at 85 to 90° C. for 30 minutes, and the major part of the phenol was finally removed by vacuum distillation at from 50 to 60° C. The remaining product was dissolved in 1 liter of toluene at 60° C. and precipitated by cooling to 20° C. The precipitate was suction filtered, washed with toluene and dried under vacuum.
Aufarbeitung
- additionwere added
- customevolved above a reaction temperature of 45° C
- stirringwith stirring
- customThe solution was then purged with nitrogen at 85 to 90° C. for 30 minutes
- customthe major part of the phenol was finally removed by vacuum distillation at from 50 to 60° C
- dissolutionThe remaining product was dissolved in 1 liter of toluene at 60° C.
- customprecipitated
- temperatureby cooling to 20° C
- filtrationfiltered
- washwashed with toluene
- customdried under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-eab9f2b47710408f940b8159016bfb8b
- Quelldatensatz
- uspto-grants-2000_04
- Patentnummer
- US06054528
Verknüpfte Notizen
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