Reacción #595304

Ecuación de reacción

methionine

→

Bis[2-(methylthio)ethyl]-2,5-piperazinedione

3,6-bis[2-(methylthio)ethyl]-2,5-piperazinedione

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.STIRRINGstirred at 160° C. for 6 hours, during which the pressure
2. 2
   Temperaturaincreased to 15 bar
3. 3
   TemperaturaThe autoclave was then cooled in an ice bath
4. 4
   Filtraciónthe resulting suspension was filtered
5. 5
   Lavadothe solid was washed with 75 ml of water
6. 6
   OtroFinally, the solid was dried in a vacuum
7. 7
   Otrodrying oven at 50° C. overnight

Procedimiento

A suspension of 13.4 g (0.09 mol) of methionine, 17.2 g (0.09 mol, purity: 91%) of methioninehydantoin (IId) and 150 g of water were introduced into a 200 ml Roth steel autoclave with magnetic stirring and stirred at 160° C. for 6 hours, during which the pressure increased to 15 bar. From time to time, the autoclave was decompressed until the pressure settled at a constant 10 bar. The autoclave was then cooled in an ice bath, and the resulting suspension was filtered and the solid was washed with 75 ml of water. Finally, the solid was dried in a vacuum drying oven at 50° C. overnight. Bis[2-(methylthio)ethyl]-2,5-piperazinedione (III) was isolated as yellowish white crystals.

Fuente