تفاعل #82899

ord-502d8aacb5dc4b6d8870e5b87a397057

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحis subsequently filtered off with suction
  2. 2
    تركيزthe filtrate is concentrated in vacuo
  3. 3
    workup.DISTILLATIONthe residue is subsequently distilled repeatedly with toluene
  4. 4
    استخلاصit is then extracted once
  5. 5
    workup.STIRRINGby shaking with water (0.3 l)
  6. 6
    أخرىthe phases are swiftly separated
  7. 7
    ترشيحThe organic phase is filtered once more
  8. 8
    تركيزconcentrated

الإجراء التجريبي

tert-Butyl bromoacetate (24 ml; 0.15 mol) is slowly added dropwise, at room temperature, to a suspension of N4 -benzoylcytosine (21.5 g; 0.1 mol) and potassium carbonate 13.8 g; 0.1 mol) in anhydrous N,N-dimethylformamide (2.15 l). The heterogeneous mixture is stirred vigorously at room temperature for 20 h and insoluble starting material is subsequently filtered off with suction; the filtrate is concentrated in vacuo and the residue is subsequently distilled repeatedly with toluene and then taken up in chloroform (1.0 l); it is then extracted once by shaking with water (0.3 l), and the phases are swiftly separated. The organic phase is filtered once more and concentrated. Yield: 15.23.g (46%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05623049uspto-grants-1997_04