HRID41626
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
H2SO4 (0.6 mL) was added to a solution of 2-bromonicotinic acid (1.5 g, 7.43 mmol, 1.00 eq.) in MeOH (20 mL). The resulting solution was stirred for 5 hours while the temperature was maintained at reflux in an oil bath. The mixture was cooled to room temperature and concentrated under vacuum. The resulting solution was diluted with EtOAc (50 mL) and the pH of the solution was adjusted to 10 with Na2CO3 (20%). The resulting organic layer was washed with water (1×50 mL) and saturated aqueous NaCl (2×100 mL), dried over anhydrous Na2SO4, and concentrated under vacuum to yield 2-bromonicotinic acid methyl ester (1.1 g) as a yellow liquid.
WORKUP
后处理
- temperaturewas maintained
- temperatureat reflux in an oil bath
- concentrationconcentrated under vacuum
- additionThe resulting solution was diluted with EtOAc (50 mL)
- washThe resulting organic layer was washed with water (1×50 mL) and saturated aqueous NaCl (2×100 mL)
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated under vacuum