반응 #595304

ord-6ccbbcd80090488ea5d8a7c08c1cd5be

반응 방정식

CSCC[C@H](N)C(=O)O
methionine
CSCCC1NC(=O)C(CCSC)NC1=O
Bis[2-(methylthio)ethyl]-2,5-piperazinedione
CSCCC1NC(=O)C(CCSC)NC1=O
3,6-bis[2-(methylthio)ethyl]-2,5-piperazinedione

시약

없음

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09095161B2uspto-grants-2015_08