As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 4316-97-6, name is 4,6-Dichloro-5-methylpyrimidine, molecular formula is C5H4Cl2N2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Computed Properties of C5H4Cl2N2
To a stirred solution of 4,6-dichloro-5-methylpyrimidine (1.0 g, 6.1 mmol), cyclopropylmethanol (0.49 g, 6.8 mmol) in THF (25 mL) is added potassium tert-butoxide (0.83 g, 7.4 mmol) at 0 oC, and the reaction mixture is stirred at 0 oC for 2 hours.The reaction mixture is added saturated aqueous NH 4Cl (20 mL) and water (80 mL), and extracted with EtOAc (80 mL).The organic layer is washed with water (80 mL x 2), and dried over sodium sulfate.Insoluble materials are separated by filtration and the filtrate is concentrated.The residue is purified by column chromatography on silica-gel eluting with n-hexane / EtOAc (99:1 to 95:5) to give 1.2 g (98% yield) of the title compound as a white solid. 1H-NMR (400 MHz, CDCl 3) delta 8.38 (1H, s), 4.27-4.18 (2H, d, J = 7.4 Hz), 2.25 (3H, s), 1.34-1.24 (1H, m), 0.65-0.59 (2H, m), 0.38-0.34 (2H, m), MS (ESI) m/z: 199 (M+H) +.
With the rapid development of chemical substances, we look forward to future research findings about 4316-97-6.
Reference:
Patent; RAQUALIA PHARMA INC.; XUANZHU PHARMA CO., LTD.; KAWAMURA, Kiyoshi; YAMAGISHI, Tatsuya; SHISHIDO, Yuji; MORITA, Mikio; YAMAGUCHI, Ryuichi; OHMI, Masashi; (182 pag.)WO2019/45035; (2019); A1;,
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