2-氯-N-(4-甲基苯基)丙烯酰胺单级连续混合悬浮-混合产物去除结晶的设计与优化,ACS Omega

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2-氯-N-(4-甲基苯基)丙烯酰胺单级连续混合悬浮-混合产物去除结晶的设计与优化
ACS Omega ( IF 3.7 ) Pub Date : 2022-04-13 , DOI: 10.1021/acsomega.1c07228
Gladys Kate Pascual ₁ , Philip Donnellan ₁ , Brian Glennon _{1,

2} , Barbara Wood _{1,

2} , Roderick C Jones ₁

Affiliation

开发了一种连续运行的单级混合悬浮-混合产物去除（MSMPR）结晶器，用于2-氯-N的连续冷却结晶-(4-甲基苯基)丙酰胺 (CNMP) 的甲苯溶液，温度为 25 至 0 °C。将前一批转化为连续工艺是开发一种将 CNMP 的合成和纯化单元操作联系起来的方法的关键，并为开发活性药物成分材料的连续工艺系列提供了进一步的见解。通过监测冷却和搅拌速率等参数如何影响粒度和产量，比较了两种批量启动策略。研究的第二部分侧重于通过确定改变停留时间和搅拌速率的影响，开发和优化与产率相关的 CNMP 在 MSMPR 结晶器中的连续冷却结晶。在 MSMPR 操作期间，聚焦光束反射率测量总计数与时间的关系曲线振荡并达到不寻常的控制状态。尽管有振荡，溶解的浓度是恒定的。正如 FTIR 数据所支持的，系统的产率和生产率在两个停留时间后保持不变。在较短的停留时间 (τ) 下总产率较高，对于 CNMP 的分离，在 τ = 20 分钟时产率为 69.51 g/h。

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Design and Optimization of the Single-Stage Continuous Mixed Suspension–Mixed Product Removal Crystallization of 2-Chloro-N-(4-methylphenyl)propenamide

A continuously operated single-stage mixed suspension–mixed product removal (MSMPR) crystallizer was developed for the continuous cooling crystallization of 2-chloro-N-(4-methylphenyl)propanamide (CNMP) in toluene from 25 to 0 °C. The conversion of the previous batch to a continuous process was key to developing a methodology linking the synthesis and purification unit operations of CNMP and gave further insight in the development of continuous process trains for active pharmaceutical ingredient materials. By monitoring how parameters such as cooling and agitation rates influence particle size and the yield, two batch start-up strategies were compared. The second part of the study focused on developing and optimizing the continuous cooling crystallization of CNMP in the MSMPR crystallizer in relation to the yield by determining the effects of varying the residence time and the agitation rates. During the MSMPR operation, the plot of the focused beam reflectance measurement total counts versus time oscillates and reaches an unusual state of control. Despite the oscillations, the dissolved concentration was constant. The yield and production rate from the system were constant after two residence times, as supported by FTIR data. The overall productivity was higher at shorter residence times (τ), and a productivity of 69.51 g/h for τ = 20 min was achieved for the isolation of CNMP.

更新日期：2022-04-13

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