反应 #2460347

ord-c91ef501761343bda4bfb84f78db4416

反应条件

温度
200°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The reaction mixture was partitioned between ethyl acetate and water
  2. 2
    萃取The reaction was extracted with ethyl acetate (×3)
  3. 3
    洗涤the combined organic layers were washed with water and saturated aqueous sodium chloride solution
  4. 4
    干燥dried over magnesium sulfate
  5. 5
    过滤After filtration
  6. 6
    浓缩the organics were concentrated in vacuo

实验过程

3-aminopyrazine-2-carbaldehyde (made in example 1(c)) (0.30 g, 2.4 mmol), N4-ethylpyridine-3,4-diamine (made in example 1(b)) (0.36 g, 2.6 mmol), and sodium hydrogensulfite (0.30 g) were combined in 3 mL of dimethylacetamide and heated to 200° C. in a SmithSynthesizer microwave for 10 minutes. The reaction mixture was partitioned between ethyl acetate and water. The reaction was extracted with ethyl acetate (×3), and the combined organic layers were washed with water and saturated aqueous sodium chloride solution, and dried over magnesium sulfate. After filtration, the organics were concentrated in vacuo. Trituration with diethyl ether affords the title compound as tan solids (0.46 g, 80%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07459454B2uspto-grants-2008_12