These common heterocyclic compound, 3972-56-3, name is 1-tert-Butyl-4-chlorobenzene, 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. HPLC of Formula: C10H13Cl
The method for synthesizing the aphid butyl fluoride ester intermediate p-tert-butyl phenylacetonitrile comprises the following steps: 1) Under argon conditions,Ethyl acetonitrile,Potassium tert-butoxide,Mix the t-butanol,Warming up to 98 ¡ã C,The control pressure is 4.5 atmospheres.Within 30min1 mol of tert-butylchlorobenzene and DMSO solution were added in 3 batches,Then control the reaction temperature to 112 ¡ã C,The reaction pressure is 5 atmospheres.The reaction ended at 2.5h.Then add deionized water,Control reaction temperature is 142¡ãC, the reaction pressure is 8 atmospheres,Continue the reaction 5h end;The ratio of 4-tert-butylchlorobenzene to ethyl cyanoacetate is 1:1.35,The amount of ethyl cyanoacetate and potassium t-butoxide is 1:1.55,The ratio of ethyl cyanoacetate to tert-butanol is 1g: 10ml,The ratio of 4-tert-butylchlorobenzene to DMSO is 1g: 5ml.The ratio of potassium t-butoxide to deionized water is 1:11.2) The system removes the solvent by a rotary evaporator.Then transfer the residue to the water,Add toluene and stir,The layers were separated, and the organic phase was collected and dried over anhydrous sodium sulfate.Then the filtrate was collected by filtration.The filtrate was distilled under reduced pressure to collect a fraction of 78 to 79 ¡ã C (0.1 torr).The product was obtained in a molar yield of 97.7percent and an HPLC purity of 98.9percent.
The synthetic route of 1-tert-Butyl-4-chlorobenzene has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shandong Nong Pharmaceutical Xue Institute; Jinan Kehai Co., Ltd.; Yang Chaohui; Fu Hongxin; Wang Ling; (6 pag.)CN109053491; (2018); A;,
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