反应详情

温度

22.5 °C

A solution of 44 g (0.3 mol) of the alcohol of Example 1 in 200 ml of methyl tert-butyl ether (MTBE) was treated at not more than 20° C. with a solution of 42.9 g of Na2Cr2O7*2H2O in 210 ml of water and 35 ml of concentrated H2SO4. After the mixture had been stirred for approximately 16 hours at 20-25° C., the phases were separated and the aqueous phase was extracted with MTBE. After washing with water and drying, the combined organic phases [lacuna] distilled. The distillation gave 34.3 g of 4-methylcyclohexyl ethyl ketone as a colorless oil of b.p.50 of 114-116° C. According to 13C NMR analysis, the ratio between the cis and trans isomers in the mixture amounted to approximately 30:70.

1. customthe phases were separated
2. extractionthe aqueous phase was extracted with MTBE
3. washAfter washing with water
4. customdrying
5. distillationthe combined organic phases [lacuna] distilled
6. distillationThe distillation