反应详情

A stirred mixture of 5.2 g. (0.02 mole) of 4-chloro-1,2-dihydro-1-methyl-2-oxo-1,8-naphthyridine-3-carboxylic acid ethyl ester, 2.0 g. (0.02 mole) of N-methylpiperazine and 2.12 g. (0.02 mole) of sodium carbonate was heated under reflux for 5 hours. The mixture was filtered and the filtrate was evaporated in a rotary evaporator. The residue was triturated with 50 ml. of a 20% aqueous sodium carbonate solution and was extracted with 50 ml. of ether. The ether layer was dried over magnesium sulfate, filtered, diluted with a few ml. of ethanol and was acidified with a saturated ethereal hydrochloric acid solution. The precipitate which formed was collected and was recrystallized from ethanol to afford 0.3 g. of product as the hydrochloride, hemihydrate, m.p. 231°-234° C. dec.

1. additionA stirred mixture of 5.2 g
2. temperatureunder reflux for 5 hours
3. filtrationThe mixture was filtered
4. customthe filtrate was evaporated in a rotary evaporator
5. customThe residue was triturated with 50 ml
6. extractionof a 20% aqueous sodium carbonate solution and was extracted with 50 ml
7. dry with materialThe ether layer was dried over magnesium sulfate
8. filtrationfiltered
9. additiondiluted with a few ml
10. customThe precipitate which formed
11. customwas collected
12. customwas recrystallized from ethanol
13. customto afford 0.3 g