تفاعل #1162471

ord-ef9ce4a2029a4382adc6774f52d90f40

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was refluxed 6.25 h
  2. 2
    درجة الحرارةcooled
  3. 3
    تركيزconcentrated in vacuo
  4. 4
    ترشيحsuction filtered
  5. 5
    غسيلthe filtrate washed with 10% aqueous sodium hydroxide (4×100 ml)
  6. 6
    أخرىRemoval of the solvent in vacuo

الإجراء التجريبي

To 92.4 g (0.646 moles) of 3-oximino-2,4-hexanedione dissolved in 807 ml of n-butanol was added 90.75 g (0.775 moles) of d,l-norvaline. The mixture was refluxed 6.25 h, then cooled and concentrated in vacuo. The residue was taken up in ethyl acetate (500 ml), suction filtered and the filtrate washed with 10% aqueous sodium hydroxide (4×100 ml). Removal of the solvent in vacuo gave 0.29 moles (48% yield based on recovered amino acid) of 4-methyl-5-propinoyl-2-propylimidazole and 5-acetyl-4-methyl-2-propylimidazole (87:13 respectively).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04395547uspto-grants-1983_07