反应详情

A mixture of 4-chloro-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid ethyl ester (EXAMPLE 68A) (50 mg, 0.22 mmol), 4-(4-chlorobenzyl)-piperidin-4-ylamine hydrochloride (65 mg, 0.22 mmol) and triethylamine (150μ) in n-butanol (1.5 mL) was irradiated in a microwave reactor (200 W) for 1 hr at 100° C. After cooling, the solvent was evaporated. The solids obtained were dissolved in ethyl acetate, the organic layer was washed with aqueous sodium hydrogen carbonate, brine and then dried (Na2SO4). Evaporation of the organic solution gave 4-[4-amino-4-(4-chlorobenzyl)-piperidin-1-yl]-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid ethyl ester as an off-white solid (80 mg, 87%). LC-MS (LCT2) m/z 415 [M+H+], Rt 3.99 min.

1. customwas irradiated in a microwave reactor (200 W) for 1 hr at 100° C
2. temperatureAfter cooling
3. customthe solvent was evaporated
4. customThe solids obtained
5. washthe organic layer was washed with aqueous sodium hydrogen carbonate, brine
6. dry with materialdried (Na2SO4)
7. customEvaporation of the organic solution