反应详情

温度

2.5 °C

An eggplant flask was charged with 5-(benzothiazol-2-yl)-2-(N,N-dimethylaminomethyl)-1-(tetrahydropyran-4-yl)benzimidazole (see Working Example 9) (0.176 g, 0.448 mmol), anhydrous diethyl ether (1 mL), and anhydrous 1,4-dioxane (7 mL), and this was stirred at 0 to 5° C. To this was added slowly a solution of hydrogen chloride in diethyl ether (2.0 M, 2 mL), after which this was stirred under these conditions for 30 minutes. The generated crystals were filtered off, these were then washed with diethyl ether (approx. 2 mL, 3 times) and dried under reduced pressure to yield the title compound (0.186 g, 96.9% yield) as a pale yellow powder.

1. stirringafter which this was stirred under these conditions for 30 minutes
2. filtrationThe generated crystals were filtered off
3. washthese were then washed with diethyl ether (approx. 2 mL, 3 times)
4. customdried under reduced pressure