تفاعل #165803

ord-04f9d786475440d3a8e31f38bff41582

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthen warmed slightly
  2. 2
    workup.ADDITIONThe mixture was poured dropwise onto water (5 ml) with rapid stirring
  3. 3
    workup.STIRRINGstirred at room temperature for 1 h
  4. 4
    ترشيحthen filtered
  5. 5
    أخرىto give a wet paste which
  6. 6
    أخرىwas dried under high vacuum at 100° C. overnight
  7. 7
    أخرىUsed directly in the next step without purification

الإجراء التجريبي

A solution of 4-[5-amino-6-(hydrazinecarbonyl)pyrazin-2-yl]-N,N-dimethyl-benzamide (100 mg, 0.3163 mmol) and 6-aminopyridine-2-carboxylic acid (43.69 mg, 0.3163 mmol) in DMF (1.000 mL) was treated with triethylamine (32.01 mg, 44.09 μL, 0.3163 mmol) then warmed slightly. The mixture was cooled to room temperature and then treated with (benzotriazol-1-yloxy-dimethylamino-methylene)-dimethyl-ammonium tetrafluoroborate (121.9 mg, 0.3796 mmol) and stirred at room temperature overnight. The mixture was poured dropwise onto water (5 ml) with rapid stirring, stirred at room temperature for 1 h then filtered to give a wet paste which was dried under high vacuum at 100° C. overnight. Used directly in the next step without purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08841308B2uspto-grants-2014_09