Citric Acid → HCID 86747321, compound

Participants

Reaction Steps

758 mg (2 mmol) of (N-t-butoxycarbonylvalyl)glycine p-nitrophenyl ester, 202 mg (2 mmol) of triethylamine and 716 mg (2 mmol) of the compound (30) obtained in Example 5 (1) were added to 10 ml of methylene chloride. The mixture solution was stirred overnight at room temperature. 10 ml of water was added to the solution and the solution was acidified with citric acid. The organic layer was separated and was removed by distillation after drying over sodium sulfate. Ethyl acetate--ether was added to the residue, the product came out of the solution, and the solid was filtered off. The solid was added to 10 mi of methanol, and 2.5 ml of 4N hydrochloride solution in dioxane was added to the solution. After the solution was stirred at room temperature for 30 minutes, the solvent was removed by distillation. The powder was filtered off and washed successively with ethanol and ether to obtain 618 mg of the subject compound (96) in a 58% yield. The results of the analysis of this compound were as follows:

Provenance & Evidence