反应详情

1-[2-(Trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-5-yl]methanamine (Intermediate 5, 75 mg, 0.349 mmol), 4-chloro-6-(1-methylethyl)pyrimidine (54.6 mg, 0.349 mmol) and DIPEA (0.122 mL, 0.697 mmol) in N-methyl-2-pyrrolidone (1 mL) were stirred in a microwave reactor at 120° C. for 1 hour. The reaction mixture was diluted with ethyl acetate (20 mL) and washed with water (10 mL), brine (10 mL), water (10 mL) and brine (10 mL). The organic layer was dried (sodium sulfate), filtered and concentrated under reduced pressure. This solid was dissolved in a mixture of acetonitrile and DMSO (1:1) (0.9 mL) and purified by MDAP (2 injections). Fractions containing pure product were combined and concentrated under reduced pressure to give the title compound as a yellow oil (28 mg);

1. washwashed with water (10 mL), brine (10 mL), water (10 mL) and brine (10 mL)
2. dry with materialThe organic layer was dried (sodium sulfate)
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. dissolutionThis solid was dissolved in a mixture of acetonitrile and DMSO (1:1) (0.9 mL)
6. custompurified by MDAP (2 injections)
7. additionFractions containing pure product
8. concentrationconcentrated under reduced pressure