Reaktionsgleichung
[N+:1]([C:4]([N+:8]([O-:10])=[O:9])(O)[CH2:5]C)([O-:3])=[O:2].[CH2:11]([CH:17]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:18]([OH:20])=[O:19])[CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].Cl[CH:30](Cl)C>>[N+:1]([C:4]([N+:8]([O-:10])=[O:9])([CH3:5])[CH2:30][O:19][C:18](=[O:20])[CH:17]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])([O-:3])=[O:2]Komponenten
4
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
Dinitropropanol (25.5 g, 0.17 mol), 2-hexyldecanoic acid (48.7 g, 0.19 mol) and 50 g of polyphosphoric acid were added to 50 mL of dichloroethane and the resulting mixture was slowly stirred using a stirrer. The solution thus obtained was slowly heated to 70° C. and then reacted for 15 hr (overnight). After the reaction, the temperature of the reactor was lowered to room temperature, and the stirrer was powered off. When the temperature of the reactor was room temperature, the dichloroethane layer was decanted, followed by extraction with a 1 N sodium hydroxide aqueous solution and then distillation under reduced pressure, affording 2,2-dinitropropyl-2-hexyldecanoate (39.6 g, yield: 60%).
Aufarbeitung
- customThe solution thus obtained
- customreacted for 15 hr (overnight)
- customAfter the reaction
- customwas lowered to room temperature
- customwas room temperature
- customthe dichloroethane layer was decanted
- extractionfollowed by extraction with a 1 N sodium hydroxide aqueous solution
- distillationdistillation under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-1ab3c6459ff0497190cbe0f2624b6bf0
- Quelldatensatz
- uspto-grants-2016_01
- Patentnummer
- US09227910B2
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