تفاعل #453715

ord-ce604a25f31d4f88833bc26b8a18e597

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITat room temperature for 16 hours
  2. 2
    استخلاصextracted with ether (150 ml)
  3. 3
    استخلاصThe organic extract
  4. 4
    غسيلwas washed with water (2×70 ml)
  5. 5
    تجفيفdried (MgSO4)
  6. 6
    أخرىevaporated in vacuo
  7. 7
    أخرىto leave a brown oil
  8. 8
    workup.DISTILLATIONThe oil was purified by distillation in vacuo (boiling point 146-147° C. @ 0.1 mmHg)

الإجراء التجريبي

Sodium hydride (1.48 g, 60% in oil) was added to a stirred solution of 3-azabicyclo[3.1.0]hexane-2,4-dione (4.0 g) and 1-iodooctane (8.88 g) in dry dimethylformamide (70 ml) under a nitrogen atmosphere at 0° C. The reaction mixture was stirred at 0° C. for a further 30 minutes and then at room temperature for 16 hours. The mixture was diluted with water (100 ml) and then extracted with ether (150 ml). The organic extract was washed with water (2×70 ml), dried (MgSO4) and evaporated in vacuo to leave a brown oil. The oil was purified by distillation in vacuo (boiling point 146-147° C. @ 0.1 mmHg) to give the title compound as a pale yellow oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06130241uspto-grants-2000_10