HRID1384226

反应详情

EQUATION

反应方程式

HRID 1384226 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureunder reflux for 1 hour
  2. customVolatile material was removed by evaporation and saturated ammonium chloride solution (20 ml)
  3. additionwas added to the residue
  4. extractionThe mixture was extracted with ethyl acetate (2×20 ml)
  5. washthe extracts were washed with water (2×15 ml)
  6. dry with materialdried (MgSO4)
  7. customThe solvent was removed by evaporation
  8. customthe residue was purified by flash chromatography
  9. washeluting with 25-50% ethyl acetate/hexane