تفاعل #1073768

معادلة التفاعل

sodium hydroxide

ethyl 6-(4-chlorophenyl)-1-methyl-2-n-propyl-4-oxonicotinate hydrochloride

→

6-(4-chlorophenyl)-1-methyl-2-n-propyl-4-oxonicotinic acid

المردود 54.0%

المذيبات

water

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture is refluxed
2. 2
   workup.WAITto stand at room temperature for 18 hrs
3. 3
   درجة الحرارة, refluxed for an additional 1 hr
4. 4
   أخرىThe solution formed
5. 5
   استخلاصis extracted with three 50 ml portions of methylene dichloride
6. 6
   أخرىThe suspension formed
7. 7
   workup.STIRRINGis stirred at room temperature for 3 hrs
8. 8
   ترشيحfiltered
9. 9
   أخرىThe filter cake is dried

الإجراء التجريبي

4.0 g (0.05 mol) of 50% aqueous sodium hydroxide is added to a suspension of 2.7 g (0.01 mol) ethyl 6-(4-chlorophenyl)-1-methyl-2-n-propyl-4-oxonicotinate hydrochloride in 50 ml of water and 10 ml of ethanol. The mixture is refluxed and stirred for 3 hrs, allowed to stand at room temperature for 18 hrs., refluxed for an additional 1 hr. and cooled to room temperature. The solution formed is extracted with three 50 ml portions of methylene dichloride and the aqueous solution is acidified to pH 1 with 12N hydrochloric acid. The suspension formed is stirred at room temperature for 3 hrs. and is vacuum filtered. The filter cake is dried to afford 1.65 g (54% yield) of 6-(4-chlorophenyl)-1-methyl-2-n-propyl-4-oxonicotinic acid, mp 184°-187° C.

المصدر