2,4-DI-Tert-butylcyclohexanol → Cyclohexanone, 2,4-bis(1,1-dimethylethyl)-
反応式
[C:1]([CH:5]1[CH2:10][CH:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:8][CH2:7][CH:6]1[OH:15])([CH3:4])([CH3:3])[CH3:2]>[Cu].[Cr]>[C:1]([CH:5]1[CH2:10][CH:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:8][CH2:7][C:6]1=[O:15])([CH3:4])([CH3:3])[CH3:2]参加物
3
実験手順
200 g (0.944 mole) of the 2,4-di-tert-butylcyclohexanol as prepared in Synthetic Example 2 and 2.0 g of a copper/chromium catalyst were introduced into a 500 ml four-necked flask and vigorously stirred therein at a temperature of 215° to 220° C. under a reduced pressure of 200 to 300 mmHg. This dehydrogenation procedure was carried out for 15 hours. After completion of the reaction, the heating and stirring were ceased and the reaction mixture was cooled to room temperature. Then the catalyst was filtered off. Thus 194 g of crude 2,4-di-tert-butylcyclohexanone having a cis/trans ratio of 81/19 was obtained. This product was rectified under reduced pressure in a Helipack packing column of a number of theoretical plates of 5 to give 158 g of 2,4-di-tert-butylcyclohexanone (b.p.: 93° to 94° C./3 mm Hg). This product had a cis/trans ratio of 85/15.