反应详情

温度

120 °C

A mixture of 1-(2-phenylethyl)-4-piperidinamine (8.17 g) and 2-chloro-N,N-dimethyl-4-pyrimidinamine (6.3 g) was stirred for 20 hours at 120° C. The reaction mixture was diluted with water and extracted with CH2Cl2. The organic layer was washed with water, dried, filtered and the solvent evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH(NH3) 96/4). The pure fractions were collected and the solvent evaporated. The residue was crystallized from CH3CN. The precipitate was filtered off and dried, yielding 3.69 g (28.4%) of N4,N4 -dimethyl-N2 -[1-(2-phenylethyl)-4-piperidinyl]-2,4-pyrimidinediamine (comp. 11).

1. extractionextracted with CH2Cl2
2. washThe organic layer was washed with water
3. customdried
4. filtrationfiltered
5. customthe solvent evaporated
6. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH(NH3) 96/4)
7. customThe pure fractions were collected
8. customthe solvent evaporated
9. customThe residue was crystallized from CH3CN
10. filtrationThe precipitate was filtered off
11. customdried