Fumaric Acid → (2R,3R)-2-(1,3-dihydroxybut-2-ylamino)-8-isopropyl-4-[4-(pyridin-2-yl)benzylamino]pyrazolo[1,5-a]-1,3,5-triazine fumarate

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Reaction Steps

The product 12 is treated with fumaric acid in an EtOH/Et2O solution. The fumaric acid salt 13 crystallizes from the reaction medium. Mp=187-189° C. 1H NMR (300 MHz, DMSO-d6): δ 13.12 (bs, 2H, OH), 8.77 (bs, 1H, NH), 8.64 (d, 1H, J=4.5 Hz, Harom), 8.03 (d, 2H, J=8.1 Hz, Harom), 7.94-7.82 (m, 2H, Harom), 7.72 (s, 1H, Harom) 7.49 (bs, 2H, Harom) r 7.35-7.31 (m, 1H, Harom), 6.62 (s, 2H, 2 ═CH), 6.06 (d, 1H, J=8.7 Hz, NH), 4.73 (bs, 2H, CH2), 4.00-3.89 (bs, 1H, CH), 3.89-3.76 (bs, 1H, CH), 3.58-3.40 (m, 2H, CH2), 2.90 (hept, 1H, J=7.0 Hz, CH), 1.22 (d, 6H, J=5.8 Hz, 2 CH3), 1.04 (bs, 3H, CH3).

Provenance & Evidence