Adding a certain compound to certain chemical reactions, such as: 766-81-4, name is 3-Bromophenylacetylene, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 766-81-4, Recommanded Product: 766-81-4
(1) by o-methyl nitrobenzene,Zinc powder, acetic acid, water, sodium nitrite, sodium azide, m-bromophenylacetylene, cuprous iodide,The molar ratio of sodium ascorbate to dimethyl sulfoxide is 1: 5: 10: 20: 1: 4: 1: 0.02: 0.1: 70,First1mmol o-nitrobenzene, 5mmol zinc powder, 10mmol acetic acid,20mmol water was added to the reactor, the reaction at room temperature for 9 hours,Subsequently, 1 mmol of sodium nitrite was added to the reactor under an ice-water bath and the reaction was continued for 10 minutes,Then 4mmol sodium azide was added and the reaction was continued for 1 hour,Finally, to the system by adding 1mmol of bromophenyl acetylene,0.02 mmol copper iodide, 0.1 mmol sodium ascorbate,70mmol dimethyl sulfoxide, the reaction 2 hours to obtain the mixed product; (2) Step (1) The resulting mixed product was diluted with 40 mL of water,Then extracted with 400mmol ethyl acetate twice,The extracts were combined and then washed with water and saturated brine each 10mL,Then dried with 2 g of anhydrous sodium sulfate,Under the conditions of a temperature of 35 C and a pressure of 0.03 MPa, the solvent was distilled off under reduced pressure to obtain a crude product,The crude product was further purified by column chromatography (300 mesh silica gel) using ethyl acetate / petroleum ether (ethyl acetate to petroleum ether 1:20 by volume) eluate to give 270 mg of product, yield 86% , The reaction equation is as follows:
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Reference:
Patent; Kunming University of Science and Technology; Jiang Yubo; Chen Zhen; Zhao Fen; Yang Rui; Xie Kai; Cheng Huiling; (10 pag.)CN104945339; (2017); B;,
Bromide – Wikipedia,
bromide – Wiktionary