反应详情

温度

75 °C

To a stirred solution of 4-[2-(4-Iodo-2-methoxy-pyridin-3-yl)-7-methyl-3H-benzoimidazol-5-yl]-piperazine-1-carboxylic acid tert-butyl ester (24 g, 43.7 mmol) was added 1,4-dioxane (750 mL) and 6 N aqueous HCl (30 mL) and the mixture was heated to 75° C. overnight. The solution was cooled to room temperature, the supernatent was poured off, and the resulting dark gummy solid was washed with anhydrous diethyl ether (3×500 mL) and dried in vacuo to give 17.7 g (93%) of the title compound as a dark solid that was used as described to prepare 4-[2-(4-Chloro-2-oxo-1,2-dihydro-pyridin-3-yl)-7-methyl-3H-benzoimidazol-5-yl]-piperazine-1-carboxylic acid tert-butyl ester and 4-[2-(4-Iodo-2-oxo-1,2-dihydro-pyridin-3-yl)-7-methyl-3H-benzoimidazol-5-yl]-piperazine-1-carboxylic acid tert-butyl ester; LCMS (M+H)+ m/z 436. (Note: A small peak (4-chloro-pyridin-2-one) in the LC/MS shows m/z 344, 346).

1. temperatureThe solution was cooled to room temperature
2. additionthe supernatent was poured off
3. washthe resulting dark gummy solid was washed with anhydrous diethyl ether (3×500 mL)
4. customdried in vacuo