With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.51674-77-2, name is 4-Chloropyrido[3,2-d]pyrimidine, molecular formula is C7H4ClN3, molecular weight is 165.58, as common compound, the synthetic route is as follows.Product Details of 51674-77-2
Intermediate 9 (700 mg, 2.06 mmol), ethyl 1-piperazineacetate (0.5 g), «-BuOH (10 mL) and DIPEA (2 mL) were combined in a sealed tube and heated at 130C for 12 days. The reaction mixture was cooled, concentrated onto silica and purified by column chromatography (Si02, 0-100% EtOAc in isohexane). The resulting material, EtOH (7 mL) and 2M HC1 in Et20 (5 mL) were combined and stirred at r.t. for 3 days. The reaction mixture was concentrated to give a pale yellow solid. A portion of this material (50 mg), «-BuOH (6 mL), DIPEA (1 mL) and 4-chloropyrido[3,2-<%yrimidine (50 mg, 0.25 mmol) were combined in a sealed tube and heated under microwave irradiation at 160C for 2 h. 15% NaOH solution (0.2 mL) was added to the reaction mixture, which was stirred at r.t. for 3 days. The mixture was concentrated to dryness and purified by preparative HPLC to give the title compound (38.1 mg) as a brown glass. 5H (DMSO-<¾) 8.93-8.85 (2H, m), 8.53 (IH, s), 8.49 (IH, s), 8.17 (IH, dd, J 8.46, 1.58 Hz), 7.90 (IH, dd, J 8.46, 4.25 Hz), 7.72 (IH, dd, J 8.91, 6.29 Hz), 7.30 (IH, t, J 9.11 Hz), 5.90-5.81 (IH, m), 3.76-3.65 (2H, m), 3.27 (2H, s), 3.25-3.17 (2H, m), 2.98-2.89 (2H, m), 2.88-2.79 (2H, m), 2.57 (3H, s), 1.64 (3H, d, J 6.69 Hz). LCMS (ES+) 476 (M+H)+, RT 2.43 minutes (Method 1)
At the same time, in my other blogs, there are other synthetic methods of this type of compound,51674-77-2, 4-Chloropyrido[3,2-d]pyrimidine, and friends who are interested can also refer to it.
Reference:
Patent; UCB PHARMA S.A.; ALLEN, Daniel, Rees; BUeRLI, Roland; HAUGHAN, Alan, Findlay; MATTEUCCI, Mizio; OWENS, Andrew, Pate; RAPHY, Gilles; SHARPE, Andrew; WO2011/58108; (2011); A1;,
Pyrimidine | C4H4N2 – PubChem,
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