反应 #4227

ord-78ad90bd69134387b5703ba1c2246b9a

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.WAITpressure for thirty minutes
  2. 2
    workup.STIRRINGwas then stirred at 50° for fifteen minutes
  3. 3
    温度The solution was then cooled in an ice bath to ~0° C
  4. 4
    过滤The solid was collected by filtration
  5. 5
    洗涤washed with water
  6. 6
    其他dried in an oven at 60° C.

实验过程

To a solution of 20 ml of concentrated nitric acid and 16 ml of concentrated sulfuric acid was added 3.9 g (0.025 mmol) of 2,6-dimethoxy-4-pyrimidinamine. The resulting solution was stirred at ambient temperature and pressure for thirty minutes and was then stirred at 50° for fifteen minutes. The solution was then cooled in an ice bath to ~0° C. The solid was collected by filtration, washed with water and dried in an oven at 60° C. to afford 3.6 g of the title compound, m.p. 178°-179° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04723991uspto-grants-1988_02