反应详情

温度

30 °C

564 (6 mol) of phenol, 10.8 g (0.12 mol) of butanethiol and 140 g (1 mol) of dihydroisophorone (3,3,5-trimethylcyclohexan-1-one) are introduced into a stirring apparatus equipped with a stirrer, thermometer, reflux condenser and gas inlet pipe at 30° C. At this temperature 44 g of 37% HCl are added. The reaction mixture is stirred for about 70 h at 28°-30° C. When 95% of the ketone has been converted (examined by GC) 2 l of water are added to the reaction mixture and a pH value of 6 is adjusted by adding a 45% NaOH solution. The reaction mixture is stirred for one hour at 80° C. and is then cooled to 25° C. The aqueous phase is decanted off and the remaining residue is washed with water at 80° C. The resulting crude product is filtered off and hot-extracted twice with n-hexane and twice with toluene and then filtered at 30° C.

1. customequipped with a stirrer
2. additionare added to the reaction mixture
3. stirringThe reaction mixture is stirred for one hour at 80° C.
4. temperatureis then cooled to 25° C
5. customThe aqueous phase is decanted off
6. washthe remaining residue is washed with water at 80° C
7. filtrationThe resulting crude product is filtered off
8. extractionhot-extracted twice with n-hexane and twice with toluene
9. filtrationfiltered at 30° C.