Fumaric Acid → 2-(1,3-Dihydroxyprop-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 17 is treated with fumaric acid in an EtOH/Et2O solution. The fumaric acid salt 18 crystallizes from the reaction medium. Mp=179-181° C. 1H NMR (300 MHz, DMSO-d6): δ 13.11 (bs, 2H, OH), 8.76 (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) 7.35-7.31 (m, 1H, Harom), 6.63 (s, 2H, 2 ═CH), 6.33 (d, 1H, J=6.0 Hz, NH), 4.67 (d, 2H, J=6.0 Hz, CH2), 3.98-3.83 (m, 1H, CH), 3.58-3.42 (m, 4H, 2 CH2), 2.91 (hept, 1H, J=7.0 Hz, CH), 1.23 (d, 6H, J=7.0 Hz, 2 CH3).

Provenance & Evidence