反应详情

温度

20 °C

2.13 g of triethylamine are added to a suspension of 1.7 g of methoxylamine hydrochloride in 40 cm3 of trichloromethane. After stirring for 15 minutes at a temperature close to 20° C., 3.69 g of ethyl 2-(2-chloro-6,7-difluoroquinoline-3-carbonyl)-3-dimethylaminoacrylate are added to the solution obtained and the mixture is stirred for 4 hours and a half at about 20° C. The reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at a temperature close to 50° C. The residue is taken up in 70 cm3 of ethanol and 3.6 g of triethylamine and the mixture is heated for 30 minutes at a temperature close to 75° C. After cooling to about 20° C., the precipitate obtained is drained and washed with 3 times 30 cm3 of ethanol. 2.67 g of 3-ethoxycarbonyl-7,8-difluoro-1-methoxy-4-oxo-1,4-dihydro-benzo[b][1,8]naphthyridine are obtained in the form of a pale yellow solid melting at 266°-268° C.

1. customclose to 20° C.
2. customobtained
3. stirringthe mixture is stirred for 4 hours
4. customat about 20° C
5. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at a temperature
6. customclose to 50° C
7. temperature3.6 g of triethylamine and the mixture is heated for 30 minutes at a temperature
8. customclose to 75° C
9. customthe precipitate obtained
10. washwashed with 3 times 30 cm3 of ethanol