تفاعل #595304

ord-6ccbbcd80090488ea5d8a7c08c1cd5be

معادلة التفاعل

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

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGstirred at 160° C. for 6 hours, during which the pressure
  2. 2
    درجة الحرارةincreased to 15 bar
  3. 3
    درجة الحرارةThe autoclave was then cooled in an ice bath
  4. 4
    ترشيحthe resulting suspension was filtered
  5. 5
    غسيلthe solid was washed with 75 ml of water
  6. 6
    أخرىFinally, the solid was dried in a vacuum
  7. 7
    أخرىdrying oven at 50° C. overnight

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09095161B2uspto-grants-2015_08