HRID1391289

反应详情

EQUATION

反应方程式

HRID 1391289 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-(Nα -carbobenzoxyglycyl-glycylamino)-4-hydroxy-4-phenyl-6-chloro-3,4-dihydroquinazoline (1.5 g) in acetic acid (20 ml) is refluxed with heating for 2 hours. The reaction mixture is evaporated under reduced pressure, and the residue is dissolved in ethyl acetate (30 ml). The ethyl acetate layer is washed with aqueous sodium bicarbonate and water in order, dried over sodium sulfate and evaporated under reduced pressure to remove the solvent. The residue is chromatographed on a column of silica gel, which is eluted with ethyl acetate/methanol to give 5-chloro-2-[3-(N-carbobenzoxyglycyl)aminomethyl-4H-1,2,4-triazol-4-yl]-benzophenone as a colorless oil (0.515 g).

WORKUP

后处理

  1. temperaturewith heating for 2 hours
  2. customThe reaction mixture is evaporated under reduced pressure
  3. dissolutionthe residue is dissolved in ethyl acetate (30 ml)
  4. washThe ethyl acetate layer is washed with aqueous sodium bicarbonate and water in order
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. customto remove the solvent
  8. customThe residue is chromatographed on a column of silica gel, which
  9. washis eluted with ethyl acetate/methanol