反应详情

温度

140 °C

A small microwave reaction vessel was charged with N-(3-(((2-chloro-5-pyrimidinyl)amino)carbonyl)-4-methylphenyl)-2-methyl-3-(trifluoromethyl)benzamide 19 (0.100 g, 0.22 mmol), pyridin-3-ylmethanamine (0.091 ml, 0.89 mmol) and IPA (1 mL). DIEA (0.058 ml, 0.33 mmol) was added and the vessel was sealed. The reaction mixture was stirred and heated in a Smith Synthesizer® microwave reactor (Personal Chemistry, Inc., Upssala, Sweden) at 140° C. for 30 min. After monitoring the reaction by LCMS and finding >95% conversion, the reaction was concentrated to dryness, and taken up in minimal CH2Cl2/MeOH. The crude reaction solution was injected onto the Isco {Redi-Sep® pre-packed silica gel column (40 g); eluent gradient: 3-80% 90/10/1 CH2Cl2/MeOH/NH3 in CH2Cl2 over 20 min} to afford pure 2-methyl-N-(4-methyl-3-(((2-((2-pyridinylmethyl)amino)-5-pyrimidinyl)amino)carbonyl)phenyl)-3-(trifluoromethyl)benzamide 21 as a white solid. MS m/z found 521.1 [MH+]; calc. for C27H23F3N6O2=520.18.

1. customA small microwave reaction vessel
2. customthe vessel was sealed
3. customthe reaction by LCMS
4. concentrationthe reaction was concentrated to dryness
5. customThe crude reaction solution