HRID1580615

反应详情

EQUATION

反应方程式

HRID 1580615 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.01 mole of 7-bromo-2,3-dihydro-5-(2-pyridyl)-2-oxo-1H-1,4-benzodiazepin-1-acetic acid methyl ester, 0.0105 mole of phosphorus pentasulfide and 100 ml. of pyridine is heated under reflux for about 24 hours. The mixture is evaporated and the residue thus obtained is dissolved in methylene chloride-water. The organic layer is separated, washed with saturated sodium bicarbonate solution, dried over anhydrous magnesium sulfate and evaporated to remove the solvent. The residue thus obtained is chromatographed on silica gel and eluted to give 7-bromo-2,3-dihydro-5-(2-pyridyl)-2-thioxo-1H-1,4-benzodiazepin-1-acetic acid methyl ester.

WORKUP

后处理

  1. temperatureunder reflux for about 24 hours
  2. customThe mixture is evaporated
  3. customthe residue thus obtained
  4. customThe organic layer is separated
  5. washwashed with saturated sodium bicarbonate solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated
  8. customto remove the solvent
  9. customThe residue thus obtained
  10. customis chromatographed on silica gel
  11. washeluted