Reference of 766545-20-4, A common heterocyclic compound, 766545-20-4, name is 2-Chloro-5,6,7,8-tetrahydro-1,6-naphthyridine hydrochloride, molecular formula is C8H10Cl2N2, 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.
15 mL of thionyl chloride was added to a solution of 0. 57 g (0.003 mol) O-trifluoromethylbenzoic acid in a reaction flask, A solution of N, N-dimethylformamide was added dropwise at room temperature with stirring, The reaction was warmed to the reflux reaction. After 2 hours, the excess amount of thionyl chloride was removed under reduced pressure, 5 mL of dichloromethane was added, This was added dropwise to a solution of 0. 40 g (0.002 mol) of 2-chloro-5, 6,7,8-tetrahydro-1,6-naphthyridine hydrochloride and 0. 41 g (0.004 mol) Triethylamine in 20 mL of dichloromethane at room temperature for 3 hours, The reaction solution was washed with 50 mL of saturated brine and the organic phase was dried over anhydrous magnesium sulfate and distilled under reduced pressure. The residue was subjected to column chromatography (ethyl acetate: petroleum ether = 1: 5 to 1: 2) to give a white Solid 0.44 g, m.p. 109.5.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Shenyang ZhonghuaPesticide Chemical R & D Co., Ltd.; YANG, JICHUN; WU, JIAO; BAN, LANFENG; XIE, YONG; SUN, QIN; LIU, ZHANGLING; (37 pag.)CN106467537; (2017); A;,
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