Optimization of Synthetic Strategy of 4鈥?鈥?5鈥?-Di-tert-butyldibenzo-18-crown-6 Using Response Surface Methodology

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• 作者：Jun Fan ; Chunhai Yi ; Xiaorong Lan ; Bolun Yang
• 刊名：Organic Process Research & Development
• 出版年：2013
• 出版时间：March 15, 2013
• 年：2013
• 卷：17
• 期：3
• 页码：368-374
• 全文大小：399K
• 年卷期：v.17,no.3(March 15, 2013)
• ISSN：1520-586X

文摘

4鈥?4鈥?5鈥?-Di-tert-butyldibenzo-18-crown-6 (DTBB18C6) was synthesized using 4-tert-butyl catechol (TBC) as starting material, 2,2鈥?diethylene glycol di(p-touenesulfonate) as cyclization reagent, Cs₂CO₃ as template, and tetrahydrofuran (THF) as solvent. The reaction was carried out in a sealed environment with nitrogen, and Cs₂CO₃ was supplemented in three steps. Response surface methodology (RSM) was used to investigate the effects of reaction temperature (X₁), initial concentration of TBC (X₂), reaction time (X₃), and Cs₂CO₃/TBC molar ratio (X₄); the experiment method was compared with published methods. From the result of RSM, the operation conditions for maximum yield, such as reaction temperature, reaction time, initial concentration of TBC, and Cs₂CO₃/TBC molar ratio were found to be 49.15 掳C, 72 h, 0.06 mol/L and 3.22, respectively. Under these optimum conditions, DTBB18C6 yield (Y) reached 43.38%.