反応 #955942

ord-7dc18e094ee14c86a438c03c7b3044c6

反応方程式

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

試薬

なし

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGstirred at 160° C. for 6 hours, during which the pressure
  2. 2
    温度increased to 15 bar
  3. 3
    温度The autoclave was then cooled in an ice bath
  4. 4
    ろ過the resulting suspension was filtered
  5. 5
    洗浄the solid was washed with 75 ml of water
  6. 6
    その他Finally, the solid was dried in a vacuum
  7. 7
    その他drying oven at 50° C. overnight

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08968817B2uspto-grants-2015_03