反应 #2439924
ord-3dc347428eed4c3f9d01dfe21c8e117c
反应方程式
3-bromo-5-pyridine-carboxylic acid
H2SO4
EtOH
→
3-bromo-5-pyridine-carboxylic acid ethyl ester
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度was refluxed for 6 hrs
- 2温度After cooling
- 3其他the solvent was removed by evaporation in vacuo
- 4workup.ADDITIONThe residue as diluted with H2O (100 ml)
- 5萃取extracted with ether (4×100 ml)
- 6洗涤The combined organic extracts were washed with saturated NaCl
- 7干燥dried over Na2SO4
- 8过滤Filtration and concentration in vacuo of the filtrate
实验过程
A stirred mixture of 3-bromo-5-pyridine-carboxylic acid (10.1 g, 50 mmol) and H2SO4 (1.5 ml) in EtOH (150 ml) was refluxed for 6 hrs. After cooling, the solvent was removed by evaporation in vacuo. The residue as diluted with H2O (100 ml), basified with 5% NaHCO3 (aq) solution and extracted with ether (4×100 ml). The combined organic extracts were washed with saturated NaCl and dried over Na2SO4. Filtration and concentration in vacuo of the filtrate yielded 3-bromo-5-pyridine-carboxylic acid ethyl ester as an oil that solidified on standing: (9.8 g, 85%).