反应详情

WSC hydrochloride (163 mg) was added to a mixture of 3′-({4-[(3,5-dioxo-1,2,4-oxadiazolidin-2-yl)methyl]phenoxy}methyl)-4-biphenylcarboxylic acid (293 mg), (2-ethoxyethyl)amine (0.11 ml), HOBt (142 mg) and DMF (10 ml), followed by stirring at room temperature for 27 hours. The solvent was evaporated under a reduced pressure, and chloroform/methanol (4/1) was added to the residue, followed by washing with water and a saturated ammonium chloride aqueous solution. The solvent was evaporated under a reduced pressure, and the residue was purified by silica gel column chromatography (chloroform/methanol), the resulting foamy substance was further crystallized by adding diethyl ether, and the resulting crystals were recrystallized from methanol to obtain 3′-({4-[(3,5-dioxo-1,2,4-oxadiazolidin-2-yl)methyl]phenoxy}methyl)-N-(2-ethoxyethyl)-4-biphenylcarboxamide (135 mg) as white crystals.

1. customThe solvent was evaporated under a reduced pressure, and chloroform/methanol (4/1)
2. additionwas added to the residue
3. washby washing with water
4. customThe solvent was evaporated under a reduced pressure
5. customthe residue was purified by silica gel column chromatography (chloroform/methanol)
6. customthe resulting foamy substance was further crystallized
7. additionby adding diethyl ether
8. customthe resulting crystals were recrystallized from methanol