反应详情

Into a two-liter, round bottom, three-necked flask equipped with a condenser, a mechanical stirrer, thermometer and a liquid addition funnel were placed 900 ml. of water, 200 g. (0.67 mole) of technical grade sodium dichromate followed by 176 g. (1.8 mole) of concentrated sulfuric acid. The contents were cooled to 55°-60° C. and 120 g. (0.94 mole) of 1-hydroxyethylcyclohexane was added over a period of 1 hour, holding the temperature between 55°-50° C. by means of external cooling. After the alcohol had been added, the reaction mixture was allowed to stir for an additional 30 minutes and then 600 ml. of water was added and the contents heated to remove the ketone by steam distillation. When no more ketone was being steam distilled, the heat was removed, the distillate of water and ketone separated and the upper organic layer was distilled under vacuum collecting the fraction boiling at 115°-116° C. There was obtained 76 g. of ketone representing a 64% yield.

1. customInto a two-liter, round bottom, three-necked flask equipped with a condenser, a mechanical stirrer
2. additionthermometer and a liquid addition funnel
3. temperatureThe contents were cooled to 55°-60° C.
4. custombetween 55°-50° C.
5. temperaturethe contents heated
6. customto remove the ketone
7. distillationby steam distillation
8. distillationdistilled
9. customthe heat was removed
10. customthe distillate of water and ketone separated
11. distillationthe upper organic layer was distilled under vacuum
12. customcollecting the fraction boiling at 115°-116° C
13. customThere was obtained 76 g