反应详情

温度

10 °C

To a solution of 2-ethoxy-1-{[2′-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl}-1H-benzimidazole-7-carboxylic acid (9.0 g) and 4-hydroxymethyl-5-methyl-1,3-dioxol-2-one (3.08 g) in N,N-dimethylacetamide (100 mL) were added p-toluenesulfonyl chloride (4.13 g), N,N-dimethylaminopyridine (0.48 g) and potassium carbonate (3.54 g) under ice-cooling and the mixture was stirred at about 10° C. for 3 hrs. After adjusting the pH of the mixture to about 5, the mixture was crystallized by adding water (72 mL) to give crystals as a solvate. The isolated crystals were suspended in a mixture of water (63 mL) and acetone (27 mL) and the suspension was stirred at about 35° C. for 2 hrs. After stirring under ice-cooling for 2 hrs, the crystals were collected by filtration and the crystals were washed with water (18 mL) and dried under reduced pressure at 40° C. to give the title compound (10.6 g, 95%).

1. temperaturecooling
2. customthe mixture was crystallized
3. additionby adding water (72 mL)
4. customto give crystals as a solvate
5. stirringthe suspension was stirred at about 35° C. for 2 hrs
6. stirringAfter stirring under ice-
7. temperaturecooling for 2 hrs
8. filtrationthe crystals were collected by filtration
9. washthe crystals were washed with water (18 mL)
10. customdried under reduced pressure at 40° C.