反应详情

The crude 2-chloro-4-{[(trans-4-heptylcyclohexyl)carbonyl]oxy}benzoic acid p-formylphenyl ester (19.1 g) obtained was dissolved in 800 ml of acetone. 30 ml of Jones' reagent were added dropwise to this solution within 15 minutes, the mixture warming slightly. The mixture was stirred for a further 40 minutes, then the separated inorganic material was filtered off under suction and the filtrate was concentrated. The residue was suspended in water and the suspension obtained was suction filtered. The residue was washed neutral with water on the suction filter and recrystallized from acetone, there being obtained 14.6 g of 2-chloro-4-{[(trans-4-heptylcyclohexyl)carbonyl]oxy}benzoic acid p-carboxyphenyl ester; m.p. (C-S) 135°-136° C., transition S-N 156° C., cl.p. (N-I) >300° C.

1. temperaturethe mixture warming slightly
2. filtrationthe separated inorganic material was filtered off under suction
3. concentrationthe filtrate was concentrated
4. customthe suspension obtained
5. filtrationfiltered
6. washThe residue was washed neutral with water on the suction
7. filtrationfilter
8. customrecrystallized from acetone, there