反应详情

A crude crystalline lincomycin A preparation contained 20% of lincomycin B; the remaining solid material was primarily A. This starting material is used for twenty 18 g runs over two Prep PAK C18 cartridges eluted isocratically with (2:1) water-methanol. Pool cuts are made. The B rich pool is concentrated to an aqueous to which enough methanol is added to make a mobile phase; this is reinjected into the Prep 500. Rich eluent from the second hpplc is concentrated as before and rechromatographed a third time. Yield: 24 g of ~99% pure lincomycin B and ca. 125 g of highly pure lincomycin A. The entire isolation scheme is outlined in Chart 2.

1. washcartridges eluted isocratically with (2:1) water-methanol
2. concentrationThe B rich pool is concentrated to an aqueous to which enough methanol
3. additionis added
4. concentrationRich eluent from the second hpplc is concentrated as before and
5. customrechromatographed a third time