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首页> 外文期刊>Crystal growth & design >Effect of temperature on antisolvent crystallization and transformation behaviors of thiazole-derivative polymorphs
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Effect of temperature on antisolvent crystallization and transformation behaviors of thiazole-derivative polymorphs

机译：温度对噻唑衍生物多晶型物反溶剂结晶和转变行为的影响

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Crystallization of the thiazole-derivative (BPT) was performed by adding water, which is an antisolvent for the solute, to methanol solutions of BPT. BPT has three polymorphs (A, B, C) and two solvates (BH(hydrate) and D(methanolate)). The effect of temperature on the polymorphic crystallization and transformation behavior was investigated in relation to the effect of the addition rate of water and the initial concentration. In the crystallization at temperatures between 333 and 313 K, the stable C form did not crystallize. At 333 K, the metastable A and BH forms crystallized competitively. At low initial concentration and slow addition rate, the A form crystallized preferentially, though at a high initial concentration and high addition rate BH tended to crystallize. It was presumed that the nucleation process of the unsolvated A form is not controlled by the dissociation equilibrium of the BH and D forms but is controlled by the kinetic process. This nucleation behavior of polymorphs at 333 K is very different from that at 323 K, which was reported previously, i.e., at low initial concentration BH crystallized, and at higher concentration the D form crystallized with BH. Furthermore, after crystallization at 333 K transformation from the BH form to the A form was observed, and it was found that the transformation rate decreases with the addition rate and the initial concentration. Such tendency is similar to that observed at 323 K. Conversely, at 313 K, the D form tended to crystallize preferentially. At low concentration the BH form also appeared with the D form, and it transformed to the D form. With a decrease of the temperature to 313 K, the D form becomes much more stable than the A and BH forms. This may accelerate preferential crystallization of the D form at 313 K.
机译：噻唑衍生物（BPT）的结晶是通过将水（作为溶质的反溶剂）添加到BPT的甲醇溶液中来进行的。 BPT具有三个多晶型物（A，B，C）和两个溶剂化物（BH（水合物）和D（甲醇盐））。研究了温度对多晶型结晶和转变行为的影响，以及水的添加速度和初始浓度的影响。在333至313 K的温度下结晶时，稳定的C形式没有结晶。在333 K时，亚稳态A和BH竞争地结晶。在低的初始浓度和缓慢的添加速率下，A晶型优先结晶，尽管在高的初始浓度和高的添加速率下BH倾向于结晶。据推测，未溶剂化的A形式的成核过程不受BH和D形式的离解平衡控制，而是受动力学过程控制。多晶型物在333 K时的成核行为与先前报道的323 K时非常不同，即在低初始浓度下BH结晶，而在较高浓度下D型则用BH结晶。此外，在333K下结晶后，观察到从BH形式向A形式的转变，并且发现转变速度随着添加速度和初始浓度而降低。这种趋势类似于在323 K下观察到的趋势。相反，在313 K下，D晶型倾向于优先结晶。在低浓度下，BH形式也与D形式一起出现，并转化为D形式。随着温度降低至313 K，D形式变得比A和BH形式稳定得多。这可以加速D形在313 K时的优先结晶。

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