反应详情

To a stirred solution of N-({1-[(4-hydroxytetrahydro-2H-pyran-4-yl)methy]piperidin-4-yl}methyl)-3-isopropyl-2-oxo-2,3-dihydro-1H-benzimidazole-1-carboxamide 1.51 g (3.51 mmol) in ethyl acetate (10 mL) and methanol (10 mL) was added a solution of 1,2-ethanedisulfonic acid dihydrate 397 mg (1.75 mmol) in methanol (5.0 mL) and the resulting suspension was stirred for 5 h at room temperatute. The mixture was filtered and the first crop was dried under vacuum for 5 h at 100° C. to give 1.78 g of crude product. 1.61 g of the crude product was dissolved in methanol (20 mL) and ethyl acetate (20 mL) was added to the solution. The resulting suspension was stirred for 2 h at room temperatute. The mixture was filtered and the crop was dried under vacuum for 4 h at 100° C. to give the titled compound 1.13 g (61%) as colorless crystals.

1. filtrationThe mixture was filtered
2. customthe first crop was dried under vacuum for 5 h at 100° C.
3. customto give 1.78 g of crude product
4. stirringThe resulting suspension was stirred for 2 h at room temperatute
5. filtrationThe mixture was filtered
6. customthe crop was dried under vacuum for 4 h at 100° C.