Hydrochloric Acid → HCID 131712097, compound

Participants

Reaction Steps

As in step A of Example 1A, 2.0 g of Boc-Tyr-DAla-Phe-Met-OCH3 was treated with HCl, anisole, EtOAC to give H-Tyr-DAla-Phe-Met-OCH3.HCl which was dissolved in 40 ml of water, methanol, acetic acid (94:5:1) and applied to a column (2.5×100 cm) of C18Hi+Flosil (80-100 mesh, Applied Science Laboratories, Inc.). The sample was eluted at 3 ml/min with a convex gradient formed from 2 liters of water, methanol, acetic acid (94:5:1) into which was fed methanol, water, acetic acid (50:49:1). The solid resulting from the evaporation of the product peak was dissolved in 10 ml of isopropanol and diluted with 100 ml of hexane to give 1.27 g (68%) of H-Tyr-DAla-Phe-Met-OCH3.HOAc, m.p. 64°-65° C., [α]D26 =10.57°, (c, 1.01 in methanol).

Provenance & Evidence