Hydrochloric Acid → HCID 131711689, compound

Participants

Reaction Steps

6.0 g (88.8 mmoles) of BOC-Trp-Met-Asp-D-Phg-NH2, prepared as described in Example 1, Step 7, are treated with 60 ml of a dioxane solution of hydrochloric acid in the presence of 3.1 ml (44 mmoles) of mercaptoethanol. After 15 minutes the reaction mixture is diluted with dry ether, and the separated solids are filtered off. The resulting 6.23 g. of hydrochloride, containing a large excess of hydrochloric acid, is suspended in 150 ml of water, the suspension is neutralized (pH=7) with triethylamine, stirred, and the precipitate is filtered off and washed with water. 4.0 g (78%) of H-Trp-Met-Asp-D-Phg-NH2 are obtained; m.p.: 230°-232° C. (decomposition); Rf7 =0.3.

Provenance & Evidence