Here, a large-scale feasible, chromatography-free process to purge triphenylphosphine oxide (TPPO) from the crude product of Mitsunobu and Wittig reactions has been developed. Divergence in physicochemical properties like polarity and solubility of TPPO against the product was utilized to precipitate TPPO directly from the reaction mixture and eliminate by simple filtration on a kilogram scale at a pilot plant with high purity of the product.
A large-scale synthesis process of N-Boc-4-fluoro-l-proline (1) from N-Boc-4-hydroxy-l-proline methyl ester (2) using nosyl fluoride
(13) as a deoxyfluorinating agent has been developed.
An eco-friendly and large-scale feasible process using a single solvent
was developed to afford moderate yields of products with excellent
purity >99% by high-performance liquid chromatography . The key
feature
of the optimization involving chromatography-free purification and
isolation on a kilogram-scale at a pilot plant scale is described.
Levonadifloxacin
(WCK 771) is a novel broad-spectrum anti-methicillin-resistant Staphylococcus aureus (MRSA) agent recently launched
in India. Five process impurities and one degradation impurity were
synthesized as reference standards for their quantification by high-performance
liquid chromatography (HPLC) methodology in drug substance and drug
product. These compounds are not easily commercially available. The
synthesis and characterization of these impurities are discussed in
detail.
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