Sodium Hydroxide → Micafungin sodium

Participants

Reaction Steps

According to the purification process for micafungin in WO2004014879, ion exchange was applied to 0.5 g of compound of formula I by using 50 ml of cation exchange resin UBK510L. The product was sampled and analyzed. HPLC purity was determined as 99.54%. Then, at room temperature, 0.1 mol/L NaOH solution was slowly added dropwise with stirring, until the pH of the solution achieving 4.0. The product was sampled and analyzed. HPLC purity was determined as 98.01% (See FIG. 2). 0.1 mol/L NaOH solution was continually added dropwise until the pH achieving 4.5. The produce was sampled and analyzed. HPLC purity was determined as 97.90%. 0.1 mol/L NaOH solution was continually added dropwise till the solution pH achieving 5.0. The product was sampled and analyzed. HPLC purity was determined as 97.81%. 0.1 mol/L NaOH solution was continually added dropwise till the solution pH achieving 5.5. The product was sampled and analyzed. HPLC purity was determined as 97.75%. 0.1 mol/L NaOH solution was continually added dropwise till the solution pH achieving 6.0. The product was sampled and analyzed. HPLC purity was determined as 97.67%. 0.1 mol/L NaOH solution was continually added dropwise until the solution pH achieving 6.5. The product was sampled and analyzed. HPLC purity was determined as 97.59%. 0.1 mol/L NaOH solution was continually added dropwise until the solution pH achieving 7.0. The product was sampled and analyzed. HPLC purity was determined as 97.30%, as shown in FIG. 3.

Provenance & Evidence