588-96-5, name is p-Bromophenetole, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Computed Properties of C8H9BrO
5.0 g of 4-bromophenylethyl ether and 100 mL of anisole were mixed and stirred until clear. spare. Add 0.72g of magnesium turnings and 100mL of anisole in turn, stir and mix thoroughly, pour 20mL of 4-bromophenethyl ether anisole solution into it, heat up to 47 C, reach the specified temperature, stop stirring, add 0.63 g of elemental iodine particles initiated the reaction and there was bubble overflow at the bottom of the system. When a large amount of air bubbles overflow, start stirring and stir slowly until the system turns from deep red to colorless, clear and transparent, and the temperature of the system is significantly improved. After adding 0.63 g of elemental iodine particles, the normal rotation speed was resumed, and the remaining 4-bromophenylethyl ether anisole solution was started to be added dropwise, and the temperature of the system was maintained at a micro reflux state, and the dropwise addition was completed in 1.2 hours. After the completion of the dropwise addition, the micro reflux reaction was maintained for 2 hours. The heating was stopped, the temperature was lowered to 3 C, and 0.47 g of cuprous iodide was added to the reaction vessel, and the temperature was further lowered to -18 C.9.96 g of 2-(bromomethyl)-4-iodochlorobenzene was mixed in 100 mL of anisole for use.When step (3) reaches the specified temperature of -18 C, slowly add 2-(bromomethyl)-4-iodochlorobenzene in anisole solution, and there is obvious temperature rise process in the middle stage before the dropwise addition, control The reaction system was reacted at -18 C. The temperature increase during the late addition was not obvious, and the addition was completed in 2.2 hours. After the dropwise addition was completed, the mixture was stirred for 2 hours. The cooling was stopped, and the temperature was naturally raised to room temperature, and stirring was continued for 12 hours. The system was quenched with 1N aqueous HCl.Concentrate to a small volume until crystallized, filter, and filter cake washed with pure water and blast dried. Weighed to obtain the target product (the yield of the product 1-chloro-2-(4-ethoxybenzyl)-4-iodobenzene was 8.94 g, the purity was 99.5%, and the yield was 95.9%)
The synthetic route of 588-96-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Nanjing Hongshan Biological Technology Co., Ltd.; Wu Fahao; Li Gang; Gao Yangzhe; (8 pag.)CN109232199; (2019); A;,
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