反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of N-(isobutoxycarbonyl)-2-(4-methoxycarbonylphenyl)-N-(3-methoxy-5-methylpyrazin-2-yl)pyridine-3-sulphonamide (830 mg) and sodium methoxide (433 mg) in methanol (25 ml) was heated under reflux for 1 hour. Volatile material was removed by evaporation and saturated ammonium chloride solution (20 ml) was added to the residue. The mixture was extracted with ethyl acetate (2×20 ml) and the extracts were washed with water (2×15 ml) and dried (MgSO4). The solvent was removed by evaporation and the residue was purified by flash chromatography, eluting with 25-50% ethyl acetate/hexane, to give 2-(4-methoxycarbonylphenyl)-N-(3-methoxy-5-methylpyrazin-2-yl)pyridine-3-sulphonamide (190 mg), m.p. 144-146° C.; microanalysis found: C, 55.2; H, 4.3; N, 13.3%; C23H24BrN4O4S requires: C, 55.1; H, 4.4; N, 13.5%.
WORKUP
后处理
- temperatureunder reflux for 1 hour
- customVolatile material was removed by evaporation and saturated ammonium chloride solution (20 ml)
- additionwas added to the residue
- extractionThe mixture was extracted with ethyl acetate (2×20 ml)
- washthe extracts were washed with water (2×15 ml)
- dry with materialdried (MgSO4)
- customThe solvent was removed by evaporation
- customthe residue was purified by flash chromatography
- washeluting with 25-50% ethyl acetate/hexane