تفاعل #96228

معادلة التفاعل

hydrochloric acid

sodium

diethyl malonate

1-methyl-1H-4H-pyrido[2,3-d][1,3]-oxazine-2,4-dione

→

4-hydroxy-1,2-dihydro-1-methyl-2-oxo-1,8-naphthyridine-3-carboxylic acid, ethyl ester

المذيبات

ethanol

water

ظروف التفاعل

المعالجة

1. 1
   أخرىwas evaporated in a rotary evaporator
2. 2
   workup.DISSOLUTIONThe residue was dissolved in 30 ml
3. 3
   درجة الحرارةThe mixture was heated
4. 4
   درجة الحرارةunder reflux for 10 minutes
5. 5
   workup.DISSOLUTIONthe thick mixture was dissolved in 100 ml
6. 6
   أخرىthe precipitate which formed
7. 7
   أخرىwas collected
8. 8
   أخرىair dried
9. 9
   أخرىwas recrystallized from ethanol

الإجراء التجريبي

To a solution of 0.345 g. (0.15 g. atom) of sodium in 30 ml. of ethanol was added 4.8 g. of diethyl malonate. The mixture was stirred at room temperature for 5 minutes and then was evaporated in a rotary evaporator. The residue was dissolved in 30 ml. of N,N-dimethylformamide and 2.67 g. (0.015 mole) of 1-methyl-1H-4H-pyrido[2,3-d][1,3]-oxazine-2,4-dione was added. The mixture was heated under reflux for 10 minutes and the thick mixture was dissolved in 100 ml. of water. The solution was acidified with conc. hydrochloric acid and the precipitate which formed was collected, air dried, and a small amount of this 1.7 g. was recrystallized from ethanol to give the analytical sample of 4-hydroxy-1,2-dihydro-1-methyl-2-oxo-1,8-naphthyridine-3-carboxylic acid, ethyl ester, m.p. 158°-160° C.

المصدر