反应详情

A solution of 22.3 g. (0.177 mole) of cycloheptan-1,3-dione and 600 mg. (3.16 mmoles) of p-toluenesulfonic acid monohydrate in 86 ml. of ethanol and 250 ml. of toluene was heated at reflux for 18 hours. A soxhlet extractor filled with molecular sieves (3 Å) was used to remove water from the reaction. The reaction was cooled, added to 800 ml. saturated sodium chloride and extracted with four 800 ml. portions of ether. The combined organic extract was dried over magnesium sulfate and evaporated to an oil. Distillation of the crude oil gave 25.3 g. (93%) of the title compound as an oil.

1. temperatureat reflux for 18 hours
2. additionA soxhlet extractor filled with molecular sieves (3 Å)
3. customto remove water
4. customfrom the reaction
5. temperatureThe reaction was cooled
6. additionadded to 800 ml
7. extractionsaturated sodium chloride and extracted with four 800 ml
8. extractionThe combined organic extract
9. dry with materialwas dried over magnesium sulfate
10. customevaporated to an oil
11. distillationDistillation of the crude oil
12. customgave 25.3 g