Min Su, Hua Sun, Qing Lu
Aug 21, 2017
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Influential Citations
2
Citations
Journal
Organic Process Research & Development
Abstract
2,2,6,6-Tetramethyl-4-piperidinol (TMP) crystal is a very important intermediate in organic synthesis. To obtain an improved crystallization yield and desirable crystal-size characteristics, several commonly used organic solvents were investigated to determine the solubility of TMP using a gravimetric method. An ethanol solvent and a cooling crystallization method were chosen to obtain an improved theroretical yield. The cooling crystallization process of TMP in the ethanol solution was further optimized to crystallize larger crystals with a narrow crystal-size distribution using an orthogonal array design. Final TMP crystals with an average diameter of 1110 μm and a diameter span of 0.715 were obtained under laboratory conditions using the optimized process.