反应详情

Ethyl 2-ethyl-3-{2'-(1-trityl-1H-tetrazol-5-yl)biphenyl-4-yl}methyl-4,5,6,7-tetrahydroimidazo[4,5-c]-pyridine-4-carboxylate (1.94 g), monoethyl malonate (0.74 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.80 g), and triethylamine (1.40 g) are dissolved in dichloromethane (20 ml). The mixture is stirred overnight at room temperature. The reaction mixture is washed with water, dried over sodium sulfate, and then evaporated to remove the solvent. The residue is dissolved in ethanol (30 ml) and thereto is added fumaric acid (2.00 g). The mixture is refluxed for three hours and evaporated to remove the solvent. The resulting residue is treated with a saturated sodium hydrogen carbonate solution and extracted with chloroform. The organic layer is dried and evaporated to remove the solvent. The resulting residue is purified by silica gel column chromatography (solvent; chloroform/methanol) to give ethyl 2-ethyl-3-{2'-(1H-tetrazol-5-yl)biphenyl-4-yl}methyl-5-ethoxycarbonylacetyl-4,5,6,7-tetrahydroimidazo[4,5-c]pyridine-4-carboxylate (1.07 g) as foam.

1. washThe reaction mixture is washed with water
2. dry with materialdried over sodium sulfate
3. customevaporated
4. customto remove the solvent
5. dissolutionThe residue is dissolved in ethanol (30 ml)
6. additionis added fumaric acid (2.00 g)
7. temperatureThe mixture is refluxed for three hours
8. customevaporated
9. customto remove the solvent
10. additionThe resulting residue is treated with a saturated sodium hydrogen carbonate solution
11. extractionextracted with chloroform
12. customThe organic layer is dried
13. customevaporated
14. customto remove the solvent
15. customThe resulting residue is purified by silica gel column chromatography (solvent; chloroform/methanol)