HRID925536

反应详情

EQUATION

反应方程式

HRID 925536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The above N-(6-amino-2,4-dioxo-3-propyl-1,2,3,4-tetrahydro-pyrimidin-5-yl)-4-benzyloxy-benzamide (1.0 g, 0.0025 mol) and phosphorous pentachloride (0.64 g, 0.0025 mol) were taken in phosphorous oxy chloride (25 ml) and refluxed for 20 hours The mixture was cooled and solvent was removed. The residue was dissolved in water (20 ml) and extracted with DCM. (3×5 ml). The organic layer was washed with sat. NaHCO3 (30 ml) followed by saturated brine solution (2×30 ml) and dried over Na2SO4. Solvent was removed and the residue was further purified by column chromatography to obtain pure 8-(4-benzyloxy-phenyl)-2-chloro-1-propyl-1,7-dihydro-purin-6-one (0.298 g, 30%) as a yellow solid.

WORKUP

后处理

  1. temperaturerefluxed for 20 hours The mixture
  2. temperaturewas cooled
  3. customsolvent was removed
  4. dissolutionThe residue was dissolved in water (20 ml)
  5. extractionextracted with DCM
  6. washThe organic layer was washed with sat. NaHCO3 (30 ml)
  7. dry with materialdried over Na2SO4
  8. customSolvent was removed
  9. customthe residue was further purified by column chromatography