تفاعل #50139

معادلة التفاعل

compound

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

diketene

→

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

المردود 49.2%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىThe mixture is evaporated under reduced pressure
2. 2
   أخرىto remove the solvent
3. 3
   workup.ADDITIONto the residue is added chloroform
4. 4
   غسيلThe mixture is washed
5. 5
   أخرىdried
6. 6
   أخرىevaporated under reduced pressure
7. 7
   أخرىThe resulting residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate/methanol=10:10:1)

الإجراء التجريبي

To a mixture of the compound obtained in Example 3 (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 mixture is evaporated under reduced pressure to remove the solvent, and to the residue is added chloroform. The mixture is washed, dried and evaporated under reduced pressure. The resulting residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate/methanol=10:10:1) 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 a foam.

المصدر