HRID373222

反应详情

EQUATION

反应方程式

HRID 373222 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Chloro-3-propyl-1-[[2'-(N-trityltetrazol-5-yl)-biphenyl-4-yl]methyl]pyrimidine-2,4(1H,3H)-dione (0.8 g) was dissolved in a solution of sodium metal (69 mg) in ethanol (10 mL) and the mixture was heated under reflux for 14 hours with stirring. The reaction mixture was concentrated to dryness and the resulting residue was dissolved in methylene chloride-water. The solution was acidified with 1N hydrochloric acid (1.5 ml), extracted and the organic layer was separated. The organic layer was washed with water, dried, and evaporated to dryness. The resulting residue was purified by column chromatography on silica gel to give white amorphous powders (0.36 g, 69%). M.p. 108°-119° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 14 hours
  3. concentrationThe reaction mixture was concentrated to dryness
  4. dissolutionthe resulting residue was dissolved in methylene chloride-water
  5. extractionextracted
  6. customthe organic layer was separated
  7. washThe organic layer was washed with water
  8. customdried
  9. customevaporated to dryness
  10. customThe resulting residue was purified by column chromatography on silica gel