Reference of 7025-06-1, A common heterocyclic compound, 7025-06-1, name is 1-Bromo-2-phenoxybenzene, molecular formula is C12H9BrO, 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.
Preparation of intermediate C01-A: 1-bromodiphenyl ether (2.49 g, 0.01 mol) was dissolved in 100 mL of dry tetrahydrofuran under nitrogen atmosphere, when the internal temperature of the system was lowered to -75 C,Slowly add 4.8 mL of n-hexane solution of n-butyllithium (2.5 mol/L).After the completion of the dropwise addition, the reaction was kept at -75 C for 2 h, and the temperature was maintained.Add 9,9-dimethyl-5H,9H-quinoline[3,2,1-de]acridone solid(2.80g, 0.009 mol), add the insulation reaction for 2h, keep warm,The reaction was continued at room temperature for 2 h, after which 70 g of a 10% by mass dilute hydrochloric acid was added dropwise.Stir for 1 h, separate the liquid, collect the organic phase, remove the solvent, and obtain 5 g of oil;Further, 60 g of glacial acetic acid and 1.0 g of concentrated hydrochloric acid having a concentration of 36.5 wt% were added to the obtained oil.The temperature was raised to reflux, the reaction was kept for 5 hours, the temperature was lowered to 25 C, and 50 g of toluene and 100 g of water were added.The liquid phase is separated, the organic phase is desolvated, the crude oil is passed through a silica gel column, and the petroleum ether is rinsed. The column liquid containing a single product component is collected, and 50 g of petroleum ether is beaten after desolvation, and the filter cake is collected by suction filtration.Obtaining intermediate C01-A,White solid powder 2.52g,Yield 60.4%.
The synthetic route of 7025-06-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; CECEP Wanrun Co., Ltd.; Gao Shukun; Zhang Jiangfeng; Sheng Lei; Li Peng; Ma Yongjie; Qin Yuhu; (20 pag.)CN109970775; (2019); A;,
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