반응 #44258

반응 방정식

2,6-dichloro-5-fluoronicotinic acid

NaOH

HCl

→

desired product

수율 47.0%

2-chloro-5-fluoro-6-oxo-1,6-dihydropyridine-3-carboxylic acid

수율 47.0%

반응 조건

후처리

1. 1
   온도at reflux for 2 hours
2. 2
   온도The mixture was cooled for 30 minutes in an ice bath
3. 3
   여과the solid filtered
4. 4
   세척washed with H2O
5. 5
   여과filtered
6. 6
   세척washed with warm EtOH
7. 7
   기타The solids were collected
8. 8
   기타dried under vacuum overnight

실험 절차

A mixture of 2,6-dichloro-5-fluoronicotinic acid (15.00 g, 71.43 mmol, Lancaster Synthesis) and 2 N NaOH (178.6 ml, 357.2 mmol) was stirred at reflux for 2 hours and then at room temperature for 16 hours. The reaction mixture was cooled to 0° C. and acidified with 12 N HCl (32.74 ml, 392.9 mmol). The mixture was cooled for 30 minutes in an ice bath, the solid filtered and washed with H2O. The isolated solid was slurried in warm EtOH, filtered and then washed with warm EtOH. The solids were collected and dried under vacuum overnight to yield the desired product (6.4 g, 47%) as a beige solid.

출처