반응 #55029

반응 방정식

hydrogen

thiophene

cyclopentanone

N-(4-piperidinyl)-2-pyrimidinamine

→

N-(1-cyclopentyl-4-piperidinyl)-2-pyrimidinamine

용매

methanol

ethanol

반응 조건

후처리

1. 1
   여과the catalyst is filtered off
2. 2
   기타the filtrate is evaporated
3. 3
   세척The whole is washed twice with a diluted sodium hydroxide solution
4. 4
   기타dried
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타The residue is crystallized from 2,2'-oxybispropane
8. 8
   여과The product is filtered off
9. 9
   기타dried

실험 절차

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.

출처