2-(Dicyclohexylphosphino)biphenyl → N2-(3-Methoxy-4-(6-methylpyridazin-4-yl)phenyl)-N4-methyl-6-((2,2,2-trifluoroethoxy)-methyl)pyrimidine-2,4-diamine

온도

120 °C

A mixture of 2-chloro-N-methyl-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-4-amine (50 mg, 0.20 mmol), 3-methoxy-4-(6-methylpyridazin-4-yl)aniline (42 mg, 0.20 mmol), cesium rbonate (127 mg, 0.39 mmol), palladium (II) acetate (7 mg, 0.03 mmol) and 2-(dicyclohexylphosphino)-biphenyl (10 mg, 0.03 mmol) in dioxane (2 mL) was heated under argon at 120° C. for 90 minutes in a microwave reactor. 2-Chloro-N-methyl-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-4-amine (72 mg, 0.28 mmol, 1.4 eq), palladium(II) acetate (7 mg) and 2-(dicyclohexylphosphino)biphenyl (10 mg) was added and the mixture was heated at 120° C. for 90 minutes in a microwave reactor. The mixture was filtered through a short silica gel plug which was washed with 10% solution of methanol in ethyl acetate (75 mL). The eluate was concentrated in vacuum and the residue was purified by preparative to give the title compound as a solid, 22 mg (26%).

1. temperaturethe mixture was heated at 120° C. for 90 minutes in a microwave reactor
2. filtrationThe mixture was filtered through a short silica gel plug which
3. washwas washed with 10% solution of methanol in ethyl acetate (75 mL)
4. concentrationThe eluate was concentrated in vacuum
5. customthe residue was purified by preparative

ORD 기록

ord-766617a20112464390c873db4aff3d00

출처 데이터셋

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09439904B2