反应详情

Ethyl 7-fluoro-1-[2-(S)-fluoro-1-(R)-cyclopropyl]-1,4-dihydro-8-methyl-5-nitro-4-oxoquinoline-3-carboxylate (2.50 g, 7.10 mmol) was dissolved in acetonitrile (20 ml), and after adding a 5% palladium carbon catalyst (water content: 50%, 1.0 g) thereto, it was stirred at room temperature for 20 hours under a hydrogen atmosphere at atmospheric pressure. After removing the catalyst by filtering (methanol washing), the filtrate was concentrated under a reduced pressure, and the residue obtained was dissolved in ethyl acetate (10 ml) and heated under reflux for 30 minutes. n-hexane (10 ml) was then added, and after performing heated refluxing for 30 minutes, there action solution was allowed to stand under room temperature. The precipitated crystals were then filtered out, washed with a 1:1 mixed solution of n-hexane:ethyl acetate and dried under a reduced pressure at 60° C. for 16 hours. 869 mg (38%) of the title compound was thereby obtained as a yellow powder.

1. customAfter removing the catalyst
2. filtrationby filtering (methanol washing)
3. concentrationthe filtrate was concentrated under a reduced pressure
4. customthe residue obtained
5. temperatureheated
6. temperatureunder reflux for 30 minutes
7. temperatureafter performing heated
8. temperaturerefluxing for 30 minutes
9. customto stand under room temperature
10. filtrationThe precipitated crystals were then filtered out
11. washwashed with a 1:1 mixed solution of n-hexane
12. dry with materialethyl acetate and dried under a reduced pressure at 60° C. for 16 hours