Reaktionsgleichung
[Cl-].[Al+3].[Cl-].[Cl-].[N+:5]([C:8]([N+:12]([O-:14])=[O:13])([CH3:11])CO)([O-:7])=[O:6].[O:15]1[CH2:20]CCOO1.[Al].Cl[CH2:23][Cl:24]>>[N+:5]([CH:8]([N+:12]([O-:14])=[O:13])[CH2:11][CH2:20][O:15][CH2:23][Cl:24])([O-:7])=[O:6]Komponenten
Versuchsvorschrift
8.8 grams of aluminum chloride was added rapidly to an ice-cooled solution of 9.9 g 2,2-dinitropropanol and 2.0 g trioxane in 50 ml dry dichloromethane under a nitrogen atmosphere. The mixture was stirred 2 days at room temperature, then it was poured onto crushed ice and the mixture stirred vigorously until all aluminum precipitates had dissolved (addition of some sulfuric acid may be required). The product solution was separated, the aqueous phase extracted with dichloromethane, and the extracts washed rapidly with a near saturated, ice cold sodium hydrogen carbonate solution. After drying (MgSO4) the solvent was evaporated in vacuo to give 12.0 g (92%) crude chloromethyl dinitropropyl ether, purity 98% by gas-liquid phase chromatography (GLPC). 1H NMR (CDCl3): δ2.18, s (3H); 4.49 (2, 2H); 5.44 (s,2H).
Aufarbeitung
- additionit was poured
- customonto crushed ice
- customprecipitates
- dissolutionhad dissolved (
- additionaddition of some sulfuric acid
- customThe product solution was separated
- extractionthe aqueous phase extracted with dichloromethane
- washthe extracts washed rapidly with a near saturated, ice cold sodium hydrogen carbonate solution
- dry with materialAfter drying (MgSO4) the solvent
- customwas evaporated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-23d5b09ec1284ad38c46266a52e35561
- Quelldatensatz
- uspto-grants-1984_06
- Patentnummer
- US04453021
Verknüpfte Notizen
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