反应详情

温度

70 °C

Acetic acid (2 ml) and ethanol (5 ml) are added to an N-(2-pyridylmethyl)-4-acetylamino-3-(3,4-methylenedioxybenzylamino)benzamide (0.490 g) and the solution is stirred for eight hours at 70° C. The residue obtained by reduced pressure condensation is purified using silica gel column chromatography (eluate: ethyl acetate/methanol=9/1), and crystallization is performed in ethyl acetate. The crystals are separated through filtration, dried and thus, 2-methyl-1-(3,4-methylenedioxybenzyl)-6-[(2-pyridylmethyl)carbamoyl]benzimidazole (0.270 g) is obtained. 1H-NMR (CDCl3, δ): 2.59 (3H, s), 4.78 (2H, d, J=4.8 Hz), 5.28 (2H, s), 5.93 (2H, s), 6.51 (1H, d, J=1.6 Hz), 6.55 (1H, dd, J=1.4 and 7.9 Hz), 6.72 (2H, d, J=8.0 Hz), 7.22 (1H, dd, J=6.7 and 5.0 Hz), 7.34 (1H, d, J=7.7 Hz), 7.62 (1H, br t), 7.67-7.75 (3H, m), 7.96 (1H, d, J=1.1 Hz), 8.58 (1H, d, J=4.9 Hz).

1. customThe residue obtained by reduced pressure condensation
2. customis purified
3. customsilica gel column chromatography (eluate: ethyl acetate/methanol=9/1), and crystallization
4. customThe crystals are separated through filtration
5. customdried