反应详情

温度

55 °C

In a 300-ml 4-necked flask equipped with a condenser, a thermometer, a dropping funnel, and a stirrer was placed 39 g of nitric acid (60% aqueous solution) and heated to 55° C. To the solution was added dropwise 93 g (0.60 mole) of 2,2,6-trimethylcyclohexanecarbaldehyde (4) composed of 35% of the trans-form and 65% of the cis-form synthesized in Synthesis Example 1-A) described above over a period of 2 hours. Thereafter, the reaction was carried out for 3 hours at the same temperature. Then, 100 g of toluene and 100 g of water were added to the reaction mixture at room temperature to wash with water and form an organic layer and an aqueous layer separately. The organic layer was washed thrice with 100 g of a saturated aqueous sodium chloride solution, and the toluene was distilled off under reduced pressure by means of an evaporator, to provide 101 g of crude 2,2,6-trimethylcyclohexanecarboxylic acid (5) composed of 35% of the trans-form and 65% of the cis-form.

1. customIn a 300-ml 4-necked flask equipped with a condenser
2. customsynthesized in Synthesis Example 1-A)
3. customdescribed above over a period of 2 hours
4. washto wash with water
5. customform an organic layer
6. washThe organic layer was washed thrice with 100 g of a saturated aqueous sodium chloride solution
7. distillationthe toluene was distilled off under reduced pressure by means of an evaporator