反应详情

Subsequently, 5.21 g of ethyl 1-[N-(3,4-methylenedioxyphenylcarbonyl) amino]cyclohexanecarboxylate synthesized in the above was dissolved in ethanol, and then, 16 ml of aqueous solution of 1N-sodium hydroxide was added dropwise thereto. After making heat reflux for 18 hours, the reaction solution was concentrated under reduced pressure. The residue thus obtained was dissolved in water and was washed with ether. After the resulting water layer was made acid (pH=2) by addition of 4-hydrochloric acid thereto, said layer was extracted with ethylacetate and was washed with 1N-hydrochloric acid and saturated brine. The resultant organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure, whereby 3.18 g of the captioned 1-[N-(3,4-methylenedioxyphenylcarbonyl)amino]cyclohexanecarboxylic acid was obtained in a yield of 68%.

1. temperatureAfter making heat
2. temperaturereflux for 18 hours
3. concentrationthe reaction solution was concentrated under reduced pressure
4. customThe residue thus obtained
5. washwas washed with ether
6. additionby addition of 4-hydrochloric acid
7. extractionwas extracted with ethylacetate
8. washwas washed with 1N-hydrochloric acid and saturated brine
9. dry with materialThe resultant organic layer was dried over anhydrous sodium sulfate
10. concentrationconcentrated under reduced pressure