Electric Literature of 799842-07-2 ,Some common heterocyclic compound, 799842-07-2, molecular formula is C16H19BrFN3O2S, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
Example 1 Preparation of Compound I A 2 L four-necked flask charged with 61 g of di(p-tolyl) phosphinate (compound (VII), prepared by referring to Org. Lett. 2005, 7, 4277?4280) and 1 L of tetrahydrofuran solution was cooled down to -20 C., followed by adding dropwise 109 mL of butyllithium solution (2.5 M) at the same temperature. After the addition is completed, the mixture was stirred for 30 minutes. A solution comprising N-(5-(bromomethyl)-4-(4-fluorophenyl)-6-isopropylpyrimidin-2-yl)-N-methyl methanesulfonamide (compound V) was then added dropwise while keeping the temperature at -20 C. After the addition is completed, the reaction was continued until the starting materials were completely consumed. The reaction was quenched with 1 L of water. The liquid was separated. The aqueous phase was extracted with 0.5 L of ethyl acetate. The organic phase was combined, and concentrated. The resultant solid was recrystallized in toluene to give compound I with a yield of 87%, and HPLC purity of >99%. (0045) 1H NMR (400 MHz, CDCl3) delta: 1.24 (6H, d, J=6.4 Hz), 2.38 (6H, s), 3.423.51 (7H, m), 3.87 (2H, d), 6.896.93 (2H, m), 7.107.16 (6H, m), 7.287.32 (4H, m).
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 799842-07-2, N-[5-Bromomethyl-4-(4-fluorophenyl)-6-isopropylpyrimidine-2-yl]-N-methylmethane sulfonamide, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Asymchem Laboratories (Tianjin) Co., Ltd.; Asymchem Life Science (Tianjin) Co., Ltd.; Tianjin Asymchem Pharmaceutical Co., Ltd.; Asymchem Laboratories (Fuxin) Co., Ltd.; Jilin Asymchem Laboratories Co., Ltd.; HONG, Hao; GAGE, James; LI, Jiuyuan; SHEN, Litao; ZHANG, Lei; DONG, Changming; (12 pag.)US2017/22169; (2017); A1;,
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