Triazolotriazine derivatives as a2a receptor antagonists
A triazolo and solvate technology, which is applied in the field of triazolotriazine derivatives, can solve problems such as ineffective compensation of tissue damage
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Embodiment 1
[0079] 2-(Furan-2-carboxamido)guanidine
[0080]
[0081] 2-Furohydrazide (37.80 g, 300 mmol), S-methylisothiourea sulfate (41.70 g, 150 mmol) were dissolved in NaOH aqueous solution (2%, 1.2 L), and stirred at room temperature for 72 h. After the reaction was completed, filter with suction, wash the filter cake twice with ice water, and dry it for the next step (25.25 g, 51.00% yield). 1 H NMR (500MHz, DMSO-d6) δ: 10.95(s, 1H), 7.56(s, 1H), 6.91(d, J=91.9Hz, 4H), 6.64(s, 1H), 6.45(s, 1H) .
Embodiment 2
[0083] 3-(furan-2-yl)-1H-1,2,4-triazol-5-amine
[0084]
[0085] 2-(Furan-2-carboxamido)guanidine (23.20 g, 138 mmol) was dissolved in DMF (464 mL), heated to 125° C. and stirred overnight. After cooling to room temperature, the solvent was removed under reduced pressure, DCM (200 mL) was added to the residue, and stirred for 30 min. After suction filtration, the filter cake was washed with DCM (20 mL×2), and dried to obtain the target product as a yellow solid (17.37 g, 84.00% yield). 1 H NMR (500MHz, DMSO-d6) δ: 12.13(s, 1H), 7.69(s, 1H), 6.69(d, J=1.8Hz, 1H), 6.54(dd, J=3.0, 1.7Hz, 1H) , 6.03(s, 2H).
Embodiment 2A
[0087] 3-(furan-2-yl)-1H-1,2,4-triazol-5-amine
[0088]
[0089] Sodium methoxide (171.4 g, 3172 mol) and aminoguanidine hydrochloride (175.3 g, 1586 mmol) were added into methanol (1200 mL) at 0° C. and stirred. Methyl furoate (100 g, 793 mmol) was dissolved in methanol (300 mL), and added dropwise to the above reaction solution. The reaction solution was heated to 75°C and stirred overnight. The reaction solution was filtered, and the filtrate was dissolved in water (50 mL) after being concentrated to dryness in vacuo. The pH was adjusted to 4 with 3N hydrochloric acid solution, and the precipitated solid was filtered and dried to obtain the title yellow solid compound (69.2 g, yield 58.1%). The structure was confirmed by H NMR detection. 1 H NMR (500 MHz, DMSO-d6) δ: 12.44 (s, 1H), 7.69 (d, 1H), 6.70 (d, 1H), 6.54 (dd, 1H), 6.03 (s, 2H).
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