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
To a mixture of methyl 2-n-butyl-3-{2'-(1H-tetrazol-5-yl)biphenyl-4-yl}methyl-4,5,6,7-tetrahydroimidazo[4,5-c]pyridine-4-carboxylate (0.50 g) and methanol (10 ml) is added diketene (0.20 g), and the mixture is stirred at room temperature for two hours. The solvent is distilled off under reduced pressure, and to the residue is added chloroform. The mixture is washed and dried, and evaporated under reduced pressure to remove the solvent. The resulting residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate/methanol) to give methyl 2-n-butyl-5-acetoacetyl-3-{2'-(1H-tetrazol-5-yl)biphenyl-4-yl}methyl-4,5,6,7-tetrahydroimidazo[4,5-c]-pyridine-4-carboxylate (0.29 g) as foam.
WORKUP
后处理
- distillationThe solvent is distilled off under reduced pressure
- additionto the residue is added chloroform
- washThe mixture is washed
- customdried
- customevaporated under reduced pressure
- customto remove the solvent
- customThe resulting residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate/methanol)