Reaktion #354547

Reaktionsgleichung

Methyl mercaptan

12-bromododecyl piperonyl ether

potassium hydroxide

→

13-thiatetradecyl piperonyl ether

Lösungsmittel

dimethoxyethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstige(0.032 mole) was bubbled into a solution of 13.0 g
2. 2
   workup.ADDITIONWhen all had been added the resulting mixture
3. 3
   Temperaturwas heated
4. 4
   Temperaturat reflux for 3 hours
5. 5
   TemperaturAfter cooling
6. 6
   Filtrationfiltering
7. 7
   Sonstigethe solvent was removed by evaporation
8. 8
   Filtrationfiltered
9. 9
   SonstigeThe filtrate was evaporated
10. 10
    Sonstigeto give 8.5 g

Vorschrift

Methyl mercaptan, 1.6 g. (0.032 mole) was bubbled into a solution of 13.0 g. (0.032 mole) of 12-bromododecyl piperonyl ether, and 5.6 g. (0.1 mole) of potassium hydroxide in 150 ml. of dimethoxyethane. When all had been added the resulting mixture was heated at reflux for 3 hours. After cooling and filtering, the solvent was removed by evaporation. The crude product was then dissoved in hexane and filtered. The filtrate was evaporated to give 8.5 g. of oily product. The NMR spectra was consistent with the assigned structure. The infrared spectra had strong adsorption peaks at 3.4, 3.5, 6.7, 6.95, 8.0, 9.0, 9.6, 10.6 and 12.2 microns. Analysis was as follows:

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