反应详情

To freshly distilled 3-ethylphenol (100 grams, 0.82 moles), was added aluminum turnings (1.62 grams, 0.06 moles) and the mixture was heated at 175° to 195° C. until hydrogen evolution had ceased. Ethyldisulfide (63 grams, 0.515 moles) was then added in one portion at 150° C. This mixture was then heated at 175° to 180° C. for 18 hours and then for about 7 hours at 196° C. The resulting mixture was hydrolyzed with 3 N HCl, extracted with diethylether, washed with water and dried over magnesium sulfate. Distillation of the mixture followed by a redistillation through a packed column gave, after removal of by-products and starting materials, ⟦8.15⟧ 14.0 grams of 2-ethylthio-5-ethylphenol as verified by 1H and 13C NMR.

1. temperatureThis mixture was then heated at 175° to 180° C. for 18 hours
2. extractionextracted with diethylether
3. washwashed with water
4. dry with materialdried over magnesium sulfate
5. distillationDistillation of the mixture
6. distillationfollowed by a redistillation through a packed column
7. customgave
8. customafter removal of by-products