A common heterocyclic compound, the phthalazine compound, name is Phthalazin-1(2H)-one,cas is 119-39-1, mainly used in chemical industry, its synthesis route is as follows.,119-39-1
A solution of 2H-Phthalazin-l-one (1.01 g, 5 mmol) in phosphorus oxychloride (5 mL) was stirred at 130 0C for 1.5 h. The phosphorus oxychloride was removed under reduced pressure. The residue was partitioned between water (10 mL) and methylene chloride (50 mL). The methylene chloride phase was separated, dried over MgSO4, and evaporated to give a yellow solid (1.015 g, 90%).[00139] The above crude product (83 mg, 0.50 mmol), N-methyl-4-methoxy-aniline (69 mg, 0.50 mmol) and cesium carbonate (200 mg, 0.61 mmol) were stirred in anhydrous DMF (1 mL) in a sealed tube at rt for 17 h. The reaction was diluted with water (5 mL) and extracted with EtOAc (2×20 mL). The EtOAc solution was washed with water (5 mL), dried, and evaporated to give a brown residue. The crude product was purified by column chromatography (SiO2, EtO Ac:hexanes/15-50%) to give a light yellow solid (5 mg, 4%): 1H NMR (CDCl3) 9.11 (s, IH), 7.85 (m, IH), 7.66 (m, IH), 7.48-7.47 (m, 2H), 7.40-7.10 (m, 2H)5 6.87-6.81 (m, IH), 3.80 (s, 3H), 3.63 (s, 3H).
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Reference£º
Patent; MYRIAD GENETICS, INC.; CYTOVIA, INC.; WO2006/74223; (2006); A2;,
Phthalazine – Wikipedia
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