反应详情

温度

75 °C

A mixture of chloromethylbenzene (1.9 g), intermediate 2 (3 g) and triethylamine (2.62 g) in N,N-dimethylacetamide (55 ml) was stirred for 2 hours at 75° C. The reaction mixture was poured out into ice-water and extracted with toluene. The separated organic layer was washed three times with water, dried, filtered and the solvent evaporated. The residue was dissolved in boiling petroleum ether and treated with activated charcoal. The mixture was filtered warm over dicalite, and the filtrate was concentrated. The concentrate was cooled on an ice-bath and the resulting precipitate was filtered off and dried, yielding 2.3 g (54.4%) of N2,N4,N4-trimethyl-N2-[1-(phenylmethyl)-4-piperidinyl]-2,4-pyrimidinediamine (comp. 8).

1. extractionextracted with toluene
2. washThe separated organic layer was washed three times with water
3. customdried
4. filtrationfiltered
5. customthe solvent evaporated
6. dissolutionThe residue was dissolved
7. additiontreated with activated charcoal
8. filtrationThe mixture was filtered
9. temperaturewarm over dicalite
10. concentrationthe filtrate was concentrated
11. temperatureThe concentrate was cooled on an ice-bath
12. filtrationthe resulting precipitate was filtered off
13. customdried