Reaktionsgleichung
[OH-].[Na+].[CH3:3][C:4](=[CH:7][CH3:8])[C:5]#[N:6].C(Cl)C=[C:11]([CH3:13])[CH3:12].[Cl-].[Na+].[C:17]1(C)C=CC=C[CH:18]=1>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH3:3][C:4]([CH:17]=[CH2:18])([CH2:7][CH:8]=[C:11]([CH3:13])[CH3:12])[C:5]#[N:6]Komponenten
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
Into a 1 liter 4-neck flask equipped with a stirrer, reflux cooler, and dropping funnel, 48 g (1.2 moles) of solid sodium hydroxide, 200 ml of toluene and 10 g of tetrabutyl ammonium bromide were first introduced, and heated to 70° C. Within 2 hours, a mixture of 81 g (1 mole) of 2-methyl-2-butenenitrile, and 125.4 g (1.2 moles) of prenyl chloride were added dropwise while stirring. Thereupon, the reaction mixture was further stirred for 3 hours at 75° C. For processing the reaction mixture, excess sodium hydroxide and sodium chloride formed in the reaction were first washed out with water. Then the phases were separated, and the organic phase washed with water to neutrality. After withdrawing the solvent, distillation took place in vacuo in a 30 cm. Vigreux column. The yield in desired product amounted to 62 g, ; corresponding to 41% of the theoretical.
Aufarbeitung
- customInto a 1 liter 4-neck flask equipped with a stirrer
- temperaturereflux cooler
- additionwere added dropwise
- stirringThereupon, the reaction mixture was further stirred for 3 hours at 75° C
- customformed in the reaction
- washwere first washed out with water
- customThen the phases were separated
- washthe organic phase washed with water to neutrality
- customAfter withdrawing
- distillationthe solvent, distillation
Quellen und Nachweise
- ORD-Eintrag
- ord-f730d43b1fce450c8c1488c1dc25ce6b
- Quelldatensatz
- uspto-grants-1986_11
- Patentnummer
- US04625046
Verknüpfte Notizen
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