Methylamine → HCID 11154287, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 6-chloro-2-{2-[3-(pyrid-2-yl)isoxazol-5-yl]pyrrolidin-1-yl}-4-(5-methyl-1H-pyrazol-3-ylamino)pyrimidine (Example 17) (250 mg, 0.59 mmol) and methylamine (4 ml of a 2M in methanol, 8.0 mmol) was heated at 130° C. for 90 minutes in a sealed vessel under microwave irradiation. The volatiles were removed by evaporation and the residue was purified by reverse phase HPLC using a C18 column eluting with water/acetonitrile/trifluoroacetic acid (95:5:0.2 decreasing in polarity to 0:100:0.2). Product containing fractions were combined and passed through a 50 g isolute SCX-2 ion exchange column. The column was eluted with methanol to elute any neutrals, followed by 7M methanolic ammonia to elute the product. The solvent was removed by evaporation to give the title compound (126 mg, 50%) as a yellow solid.

Provenance & Evidence