反应详情

To a stirred mixture of cyclohexanone (19.6 g.) and ethanol (50 c.c.), kept at or below 0°C, was added 1-amino-3,3,5-trimethylcyclohexyl hydroperoxide (17.3 g., 78% pure); solution was complete in ca. 10 min. To the solution was added conc. sulphuric acid (3 drops) and magnesium sulphate and the mixture was stored at 0°C for 3 days. The solid was filtered off, the filtrate washed with water, dried and distilled, to give cyclohexanone, dihydroisophorone and a fraction (11.5 g.), b.p. 90° - 100° at 0.02 mm.Hg., peroxide equivalent 179. By mass spectroscopy the product was shown to contain the unsymmetrical peroxide ##SPC32##

1. custombelow 0°C
2. waitthe mixture was stored at 0°C for 3 days
3. filtrationThe solid was filtered off
4. washthe filtrate washed with water
5. customdried
6. distillationdistilled