Effective Phosphorylation of 2,2′-Methylene-bis(4,6-di-tert-butyl) Phenol in Continuous Flow Reactors,Organic Process Research & Development

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Effective Phosphorylation of 2,2′-Methylene-bis(4,6-di-tert-butyl) Phenol in Continuous Flow Reactors
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2021-08-23 , DOI: 10.1021/acs.oprd.1c00105
Hanlin Yao ₁ , Li Wan ₁ , Xiaoyu Zhao ₁ , Yahui Guo ₁ , Jian Zhou ₁ , Xiaofan Bo ₁ , Yuxin Mao ₁ , Zhong Xin _{1,

2}

Affiliation

Nucleating agent intermediate 2,2′-methylene-bis(4,6-di-tert-butylphenol) phosphate chloride was synthesized successfully in a continuous flow by the phosphorylation reaction for the first time. After evaluating several different continuous flow reactors, the continuous Coflore agitated cell reactor (ACR) designed based on the continuous stirred-tank reactor (CSTR) principle was proved capable of overcoming the severe channel clogging caused by the precipitation product triethylamine hydrochloride. This can be attributed to the violent agitation and particle size control by the moving agitators. The yield in continuous flow after optimization reached nearly 98% at 100 °C within the residence time of only 4 min and the optimal equivalents of triethylamine and POCl₃ are 2.8 and 1.1, respectively. In contrast to the batch operation, the yield has been increased through continuous operation. This is an effective method for the synthesis of the desired product and exhibits the merits of short residence time, easy operation, and straightforward scale-up.

中文翻译：

连续流动反应器中 2,2'-亚甲基-双（4,6-二叔丁基）苯酚的有效磷酸化

首次通过磷酸化反应在连续流动中成功合成了成核剂中间体2,2'-亚甲基-双(4,6-二叔丁基苯酚)磷酸酯氯化物。在对几种不同的连续流动反应器进行评估后，证明基于连续搅拌釜反应器（CSTR）原理设计的连续 Coflore 搅拌池反应器（ACR）能够克服沉淀产物三乙胺盐酸盐引起的严重通道堵塞。这可归因于移动搅拌器的剧烈搅拌和粒度控制。优化后的连续流产率在100°C下在仅4分钟的停留时间内达到近98%，三乙胺和POCl ₃的最佳当量分别为 2.8 和 1.1。与间歇操作相比，通过连续操作提高了产量。这是合成所需产物的有效方法，具有停留时间短、操作简单和放大简单的优点。

更新日期：2021-09-17

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