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L-Methionine → 3,6-bis[2-(methylthio)ethyl]piperazine-2,5-dione

HRID 868760
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Reaktionsgleichung

Reaktionsgleichung von HRID 868760
[NH2:1][C@H:2]([C:7]([OH:9])=O)[CH2:3][CH2:4][S:5][CH3:6]>O>[CH3:6][S:5][CH2:4][CH2:3][CH:2]1[NH:1][C:7](=[O:9])[CH:2]([CH2:3][CH2:4][S:5][CH3:6])[NH:1][C:7]1=[O:9]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 6137L-Methionine

Produkt 1

HCID 1698423,6-bis[2-(methylthio)ethyl]piperazine-2,5-dione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  • stirringstirred at 160° C. for 6 hours, during which the pressure
  • temperatureincreased to 15 bar
  • temperatureThe autoclave was then cooled in an ice bath
  • filtrationthe resulting suspension was filtered
  • washthe solid was washed with 75 ml of water
  • customFinally, the solid was dried in a vacuum
  • customdrying oven at 50° C. overnight
  • Quellen und Nachweise

    ORD-Eintrag
    ord-7dc18e094ee14c86a438c03c7b3044c6
    Quelldatensatz
    uspto-grants-2015_03
    DOI
    10.6084/m9.figshare.5104873.v1
    Patentnummer
    US08968817B2

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