تفاعل #4390

ord-9d28aa19805e4a3182693ceb169ad3c2

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for 24 hours under a nitrogen atmosphere
  2. 2
    أخرىto stand at room temperature
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    غسيلThe extract was washed with water
  5. 5
    تجفيفdried over magnesium sulfate
  6. 6
    أخرىevaporated in vacuo
  7. 7
    أخرىThe residue was purified by column chromatography on silica gel (110 g) with a mixture of chloroform and methanol (100:3) as an eluent

الإجراء التجريبي

A mixture of 2-amino-3-chloropyrazine (4.3 g), 2-methylbenzylamine (4.6 g), potassium carbonate (5.5 g), and potassium iodide (0.4 g) in N,N-dimethylformamide (43 ml) was refluxed for 24 hours under a nitrogen atmosphere and allowed to stand at room temperature. The mixture was poured into water and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel (110 g) with a mixture of chloroform and methanol (100:3) as an eluent to give 2-amino-3-(2-methylbenzylamino)pyrazine (1.4 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04725601uspto-grants-1988_02