Trifluoromethanesulfonic acid → HCID 13175234, compound

Participants

Reaction Conditions

Reaction Steps

In a round-bottom flask equipped with a mechanical stirrer, a thermometer, a condenser 4.00 g (17.2 mmole) N,N′-bis(carboxymethyl)-2,5-diketopiperazine was mixed with 25 ml trifluoromethanesulfonic acid. Subsequently, the reaction mixture was heated to 75° C. and 1.89 g (8.6 mmole) tetraphosphorus hexaoxide was added slowly. Afterwards the reaction mixture was stirred for 16 hour at 75° C. During the addition and during the reaction time the evolution of carbon monoxide was observed. At ambient temperature 30 ml of water was added to the reaction mixture which subsequently was heated to 95° C. for 6 hour. A white solid precipitated that was removed by filtration at ambient temperature (yield: 4.35 g). The solid consisted of N,N′-bis(phosphonomethyl)-2,5-diketopiperazine at 98.9% by weight.

Provenance & Evidence