TY - JOUR
T1 - Effect of Acetonitrile-Based Crystallization Conditions on the Crystal Quality of Vitamin D3
AU - Gruber-Woelfler, Heidrun
AU - Escribà-Gelonch, Marc
AU - Noël, Timothy
AU - Maier, Manuel C.
AU - Hessel, Volker
PY - 2017/11/1
Y1 - 2017/11/1
N2 - To design an integrated continuous crystallization setup that is directly coupled to a photochemical synthesis in flow, the crystallization of vitamin D3 was studied in detail. Because of the high solubility of the vitamin in the reaction solvent tert-butylmethyl ether, a solvent swap to acetonitrile was necessary. While other methods use a multistep procedure, with the proposed approach, crystalline vitamin D3 can be obtained within one crystallization step. The influence of crystallization parameters, such as the initial concentration of vitamin D3, stirring as well as cooling temperature, rate, and time, on the obtained results in terms of yield, crystal shape, polymorphism, and particle size distribution are discussed in detail.
AB - To design an integrated continuous crystallization setup that is directly coupled to a photochemical synthesis in flow, the crystallization of vitamin D3 was studied in detail. Because of the high solubility of the vitamin in the reaction solvent tert-butylmethyl ether, a solvent swap to acetonitrile was necessary. While other methods use a multistep procedure, with the proposed approach, crystalline vitamin D3 can be obtained within one crystallization step. The influence of crystallization parameters, such as the initial concentration of vitamin D3, stirring as well as cooling temperature, rate, and time, on the obtained results in terms of yield, crystal shape, polymorphism, and particle size distribution are discussed in detail.
KW - Crystallization
KW - Polymorphism
KW - Solubility
KW - Vitamin D
UR - http://www.scopus.com/inward/record.url?scp=85032190933&partnerID=8YFLogxK
U2 - 10.1002/ceat.201700080
DO - 10.1002/ceat.201700080
M3 - Article
AN - SCOPUS:85032190933
SN - 0930-7516
VL - 40
SP - 2016
EP - 2024
JO - Chemical Engineering & Technology
JF - Chemical Engineering & Technology
IS - 11
ER -