HRID373222
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperatureunder reflux for 14 hours
- concentrationThe reaction mixture was concentrated to dryness
- dissolutionthe resulting residue was dissolved in methylene chloride-water
- extractionextracted
- customthe organic layer was separated
- washThe organic layer was washed with water
- customdried
- customevaporated to dryness
- customThe resulting residue was purified by column chromatography on silica gel