反应详情

2-(3,5-Bis-trifluoromethyl-phenyl)-N-methyl-N-[2-methyl-6′-(4-methyl-piperazin-1-yl)-[3,4′]bipyridinyl-3′-yl]-isobutyramide of formula I-2 can be prepared as follows: A solution of 6′-chloro-2-methyl-[3,4′]bipyridinyl-3′-carboxylic acid (VI), triethylamine and diphenylphosphoryl azide in tert-butanol is stirred at about 90° C. under argon for 1.5 h. After cooling to room temperature, the solvent is evaporated. The residue is diluted with ethyl acetate and washed with aqueous sodium hydrogencarbonate solution and brine. The organic layer is concentrated and purified to give the compound (6′-chloro-2-methyl-[3,4′]bipyridinyl-3′-yl)-carbamic acid tert-butyl ester of formula VIII.

1. customthe solvent is evaporated
2. additionThe residue is diluted with ethyl acetate
3. washwashed with aqueous sodium hydrogencarbonate solution and brine
4. concentrationThe organic layer is concentrated
5. custompurified