反应详情

温度

150 °C

A mixture of 3.4 parts of 6-chloro-3-nitro-2-pyridinamine, 7.4 parts of N-[1-(2-aminoethyl)-4-piperidinyl]-1-[(4-fluorophenyl)-methyl]-1H-benzimidazol-2-amine and 10 parts of 1-methyl-2-pyrrolidinone was stirred and heated for 2 hours at 150° C. The reaction mixture was cooled and taken up in methanol saturated with ammonia. The whole was evaporated and water was added to the residue. The product was extracted three times with 4-methyl-2-pentanone. The combined extracts were dried, filtered and evaporated in vacuo. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 4-methyl-2-pentanone, yielding 5 parts (50%) of N6 -[2-[4-[[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]-amino]-1-piperidinyl]ethyl]-3-nitro-2,6-pyridinediamine; mp. 205.7° C. (compound 63).

1. temperatureThe reaction mixture was cooled
2. customThe whole was evaporated
3. additionwater was added to the residue
4. extractionThe product was extracted three times with 4-methyl-2-pentanone
5. customThe combined extracts were dried
6. filtrationfiltered
7. customevaporated in vacuo
8. customThe residue was purified by column-chromatography over silica gel using
9. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
10. customThe pure fractions were collected
11. customthe eluent was evaporated
12. customThe residue was crystallized from 4-methyl-2-pentanone