Methanesulfonic Acid → HCID 22594096, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 2-allylamino-4-[2-methyl-5-(2-morpholinopyrid-4-ylcarbonylamino)anilino]pyrimidine (0.151 g), methanesulphonic acid (0.1 ml) and 30% palladium-on-carbon (0.034 g) in DMA (1 ml) was stirred and heated to 140° C. for 24 hours. The mixture was cooled to ambient temperature and filtered. A mixture of methylene chloride and isohexane was added to the filtrate. The resultant precipitate was isolated and purified by column chromatography on silica using a 89:10:1 mixture of methylene chloride, methanol and a saturated aqueous ammonium hydroxide solution as eluent. There was thus obtained the title compound as a solid (0.01 g); NMR Spectrum: (DMSOd6) 2.16 (s, 3H), 3.47 (m, 4H), 3.7 (m, 4H), 4.78 (br m, 4H), 5.98 (m, 1H), 7.01 (m, 1H), 7.16 (m, 2H), 7.39 (m, 1H), 7.65 (m, 1H), 7.72 (m, 1H), 8.17 (m, 1H); Mass Spectrum: M+H+ 406.

Provenance & Evidence