تفاعل #44258

معادلة التفاعل

2,6-dichloro-5-fluoronicotinic acid

NaOH

HCl

→

desired product

المردود 47.0%

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

المردود 47.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 2 hours
2. 2
   درجة الحرارةThe mixture was cooled for 30 minutes in an ice bath
3. 3
   ترشيحthe solid filtered
4. 4
   غسيلwashed with H2O
5. 5
   ترشيحfiltered
6. 6
   غسيلwashed with warm EtOH
7. 7
   أخرىThe solids were collected
8. 8
   أخرىdried under vacuum overnight

الإجراء التجريبي

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.

المصدر