Reference of 2972-52-3, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride. A new synthetic method of this compound is introduced below.
Methyl 2-(butYlaminoV4-(((tra^^ (0734) (0735) To a solution of 2,4-dichloropyrimidine-5-carbonyl chloride (500 mg, 2.38 mmol) in dichloromethane (30 mL) was added methanol (87.6 mg, 2.73 mmol) and diisopropylethylamine (369 mg, 2.86 mmol) at 0 °C. The resulting mixture was stirred for 1 h at 0 °C. Then the solvent was removed. The residue (461mg, 94percent) was dissolved in IP A (20 mL) and followed by the addition of tra5′-4-aminocyclohexanol (301.6 mg, 2.62 mmol) then DIEA (461.4 mg, 3.57 mmol) dropwisely. The resulting mixture was stirred at 0 °C for 90 min. After which butylamine (208.8 mg, 2.86 mmol) was added, followed by DIEA (461.4 mg, 3.57 mmol). The resulting mixture was stirred at room temperature for 3 h. Water was then added. The resulting mixture was extracted with EtOAc (3X). The combined organic layers were dried filtered and concentrated. The residue was purified on ISCO to provide methyl 2-(butylamino)-4-(((traj,-4-hydroxycyclohexyl)amino)pyrimidine-5 – carboxylate (682.6 mg, 89percent over 3 steps). 1H NMR (400 MHz, CDC13) delta 9.21 (s, 1H), 8.77 (s, 1H), 6.29 (s, 1H), 4.81-4.64 (m, 1H), 4.51 (s, 3H), 4.46-4.38 (m, 1H), 4.13-4.11 (m, 2H), 2.89-2.81 (m, 2H), 2.74 (d, J = 9.7 Hz, 2H), 2.35-2.25 (m, 2H), 2.23-2.00 (m, 6H), 1.67 (t, J = 7.2 Hz, 3H); 13C NMR (101 MHz, CDC13) delta 167.9, 162.5, 161.3, 160.3, 95.5, 69.7, 51.2, 48.3, 41.1, 33.8, 31.7, 30.3, 20.1, 13.8; MS m/z 323.20 [M+H]+.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,2972-52-3, 2,4-Dichloro-5-pyrimidinecarbonyl chloride, and friends who are interested can also refer to it.
Reference:
Patent; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; WANG, Xiaodong; ZHANG, Weihe; FRYE, Stephen; WO2015/157127; (2015); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia