Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) → HCID 178476967, compound

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Reaction Steps

To a stirred suspension of 4-hydroxy-2-(pyridazin-3-yl)pyrimidine-5-carboxylic acid, 30-ie, (137 mg, 0.63 mmol) in MeCN (10 mL) was added HATU (357 mg, 0.94 mmol), TEA (190 mg, 1.88 mmol) and diethyl 4-(amino(phenyl)methyl)phenylphosphonate, 2-c, (200 mg, 0.63 mmol). The solution was stirred at room temperature for 1 h. The product was precipitated from ice water (50 mL, crush ice). The product was collected by vacuum filtration and dried in a vacuum to afford a syrup, which was purified by pre-HPLC to yield title crude, 8-5, product as pale yellow (100 mg, 31%) 1H NMR (300 MHz, DMSO-d6) δ1.19-1.24 (t, J=7.5 Hz, 6H), 3.96-4.01 (q, J=7.5 Hz, 4H), 6.34-6.36 (d, J=6.0 Hz, 1H), 7.37-7.70 (m, 11H), 7.70 (m, 1H), 8.50 (m, 2H), 9.494 (d, J=3.0 Hz, 1H), 10.52 (s, 1H); LC-MS: (M+H)+ 520.

Provenance & Evidence