反应 #4390

ord-9d28aa19805e4a3182693ceb169ad3c2

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed for 24 hours under a nitrogen atmosphere
  2. 2
    其他to stand at room temperature
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    洗涤The extract was washed with water
  5. 5
    干燥dried over magnesium sulfate
  6. 6
    其他evaporated in vacuo
  7. 7
    其他The residue was purified by column chromatography on silica gel (110 g) with a mixture of chloroform and methanol (100:3) as an eluent

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04725601uspto-grants-1988_02