反応 #955942
ord-7dc18e094ee14c86a438c03c7b3044c6
反応方程式
methionine
→
Bis[2-(methylthio)ethyl]-2,5-piperazinedione
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
- 1workup.STIRRINGstirred at 160° C. for 6 hours, during which the pressure
- 2温度increased to 15 bar
- 3温度The autoclave was then cooled in an ice bath
- 4ろ過the resulting suspension was filtered
- 5洗浄the solid was washed with 75 ml of water
- 6その他Finally, the solid was dried in a vacuum
- 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.