تفاعل #56260

ord-628c7d3a1ad94e558bc41b3b4bf34f0f

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىis obtained
  2. 2
    workup.WAITthe reaction mixture is left
  3. 3
    workup.DISTILLATIONExcess tert.-butylamine is then distilled off
  4. 4
    workup.ADDITIONthe residue is mixed with methanol
  5. 5
    أخرىagain evaporated to dryness
  6. 6
    ترشيحis filtered off with suction
  7. 7
    أخرىAfter recrystallizing twice from a little methanol, there

الإجراء التجريبي

5 g of adenosine-5'-carboxylic acid methyl ester are heated together with 100 ml of tert.-butylamine on a streambath until a clear solution is obtained and thereafter the reaction mixture is left to stand for 16 hours at ambient temperature. Excess tert.-butylamine is then distilled off and the residue is mixed with methanol, again evaporated to dryness and the solid residue, after slurrying in cold methanol is filtered off with suction. After recrystallizing twice from a little methanol, there are obtained 2.15 g (38% of theory) of adenosine-5'-carboxylic acid N-tert.-butylamide, which melts, with decomposition, at 279°-280° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04224438uspto-grants-1980_09