反应 #4424

ord-dc411ea16f934b7bbc3fdf11d0029adc

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was refluxed for 3 hours
  2. 2
    其他The mixture was evaporated
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in chloroform
  4. 4
    洗涤washed with aqueous sodium bicarbonate solution
  5. 5
    干燥The organic layer was dried over magnesium sulfate
  6. 6
    其他evaporated
  7. 7
    其他The residue was chromatographed on silica gel using
  8. 8
    workup.ADDITIONa mixture of chloroform and methanol (95:5)

实验过程

To a suspension of 2-chloro-3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine (1.07 g) in ethanol (10 ml) was added piperazine (0.70 g). The mixture was refluxed for 3 hours, cooled to ambient temperature. The mixture was evaporated, and the residue was dissolved in chloroform and washed with aqueous sodium bicarbonate solution. The organic layer was dried over magnesium sulfate and evaporated. The residue was chromatographed on silica gel using a mixture of chloroform and methanol (95:5) to give 3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-2-(1-piperazinyl)-4-(2,4,6-trimethylphenylimino)pyrimidine (0.69 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04725600uspto-grants-1988_02