Hydrochloric Acid → 945667-22-1

Participants

Reaction Conditions

Reaction Steps

The compound of Boc protected (amino group protected by Di-tert-butyl dicarbonate group) saxagliptin (5.0 g gm) was dissolved in methylene chloride (40 ml); and the concentrated hydrochloric acid (4 ml) was added to the above solution. The reaction mixture was stirred for 4 hrs at 25-30° C. After the completion of the reaction, purified water (40 ml) was added to the reaction mixture at 25-30° C. and the pH was adjusted to 9-10 by the addition of potassium carbonate at the same temperature. Methylene chloride (20 ml) was added to the reaction mixture and stirred. The methylene chloride layer was separated and distilled under vacuum. The resulting residue was mixed with ethylacetate (25 ml) and treated with purified water. The contents were stirred, the resultant solid was filtered under vacuum and dried at 50-55° C. for 6 hrs. Yield: 75%.

Provenance & Evidence