反应 #55029

ord-f8d791ed86564f6688485bff2cc5b045

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the catalyst is filtered off
  2. 2
    其他the filtrate is evaporated
  3. 3
    洗涤The whole is washed twice with a diluted sodium hydroxide solution
  4. 4
    其他dried
  5. 5
    过滤filtered
  6. 6
    其他evaporated
  7. 7
    其他The residue is crystallized from 2,2'-oxybispropane
  8. 8
    过滤The product is filtered off
  9. 9
    其他dried

实验过程

To 0.5 parts of a solution of 2 parts of thiophene in 40 parts of ethanol, are added 2 parts of cyclopentanone, 5.5 parts of N-(4-piperidinyl)-2-pyrimidinamine and 120 parts of methanol. The whole is hydrogenated at normal pressure and at room temperature with 2 parts of palladium-on-charcoal 10%. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. The residue is taken up in 4-methyl-2-pentanone and a small amount of trichloromethane. The whole is washed twice with a diluted sodium hydroxide solution, dried, filtered and evaporated. The residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 2.3 parts of N-(1-cyclopentyl-4-piperidinyl)-2-pyrimidinamine; mp. 118° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04151286uspto-grants-1979_04