Reference of 1533519-85-5,Some common heterocyclic compound, 1533519-85-5, name is Methyl 2-((4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazol-3-yl)thio)acetate, molecular formula is C18H17N3O2S, 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.
In a 5L three-necked flask, add 160.0g of Intermediate 4 and 1.28L of tetrahydrofuran, start stirring, and raise the temperature to 3542.0.Stir until dissolved; lower the temperature to 2732, add 148.0g NBS, and react for 3.04.0h;Reduce the temperature to 5, add 800ml of toluene and 800ml of purified water, stir and separate the liquid, and use 800ml of 3% sodium bisulfite solution for the organic phase,Wash with 800ml of 5% sodium bicarbonate solution, let stand for liquid separation, collect the organic phase, add 580ml of 1mol/L sodium hydroxide to the organic phase, react for 2h,Separate the liquid, collect the aqueous phase, concentrate, cool the crystal, filter, and wash with water to obtain a wet product; add 720ml of purified water to the wet product,Heat to 35, stir to dissolve, add 1.6L of ethyl acetate, adjust the system pH=24 with 24% hydrobromic acid, stir for 30min,Separate the liquid, wash the organic phase once with 320ml of purified water, concentrate the organic phase until the solid precipitates,Keep warm at 3842, continue to stir and crystallize for 34h, then slowly reduce the temperature to 510, stir for 2h,Filtration, washing, and vacuum drying under reduced pressure to obtain 123.0 g of crude Recinald. The purity is 95.12%,
The synthetic route of 1533519-85-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Beijing Xinkaiyuan Pharmaceutical Technology Co., Ltd. Hainan Fen Corporation; Xia Zhongning; Wu Jin; Zhang Lijie; (8 pag.)CN111153862; (2020); A;,
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