Реакция #354547

Уравнение реакции

Methyl mercaptan

12-bromododecyl piperonyl ether

potassium hydroxide

→

13-thiatetradecyl piperonyl ether

Растворители

dimethoxyethane

Условия реакции

Обработка

1. 1
   Другое(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
   Температураwas heated
4. 4
   Температураat reflux for 3 hours
5. 5
   ТемператураAfter cooling
6. 6
   Фильтрацияfiltering
7. 7
   Другоеthe solvent was removed by evaporation
8. 8
   Фильтрацияfiltered
9. 9
   ДругоеThe filtrate was evaporated
10. 10
    Другоеto give 8.5 g

Методика

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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