تفاعل #366752

معادلة التفاعل

2-chloro-6-methyl-4-pyridinecarboxylic acid

ethanol

→

ethyl 2-chloro-6-methyl-4-pyridinecarboxylate

المردود 86.0%

المذيبات

sulphuric acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 2 hours
2. 2
   أخرىThe volatiles were removed by evaporation
3. 3
   workup.DISSOLUTIONthe residue was dissolved in methylene chloride
4. 4
   غسيلThe solution was washed with a saturated aqueous sodium hydrogen carbonate solution and brine
5. 5
   تجفيفdried (MgSO4)
6. 6
   أخرىthe solvent removed by evaporation
7. 7
   أخرىThe residue was purified by column chromatography
8. 8
   غسيلeluting with ethyl acetate/petroleum ether (1/9)

الإجراء التجريبي

A solution of 2-chloro-6-methyl-4-pyridinecarboxylic acid (2 g, 12 mmol) in ethanol (100 ml) and concentrated sulphuric acid (10 ml) was heated at reflux for 2 hours. The volatiles were removed by evaporation and the residue was dissolved in methylene chloride. The solution was washed with a saturated aqueous sodium hydrogen carbonate solution and brine, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by column chromatography eluting with ethyl acetate/petroleum ether (1/9) to give ethyl 2-chloro-6-methyl-4-pyridinecarboxylate (2 g, 86%).

المصدر