反应详情

温度

110 °C

A mixture of 0.16 g of 10-[(6-chloro-3-pyridinyl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.5 ml of benzylamine and 0.2 ml of N,N'-dimethylpropyleneurea is stirred and heated at 110° C. for 7 hours. After cooling to room temperature, the mixture is washed with hexane (3 times 10 ml). The residue is dissolved in water and made alkaline with 1N NaOH. The suspension is washed with H2O and extracted with ethyl acetate. The organic extract is washed with brine, dried (Na2SO4) and filtered through a thin pad of hydrous magnesium silicate. The filtrate is evaporated and the residue triturated with diethyl ether-hexane to give 0.20 g of white solid; mass spectrum (CI) 395 (M+H).

1. temperatureAfter cooling to room temperature
2. washthe mixture is washed with hexane (3 times 10 ml)
3. dissolutionThe residue is dissolved in water
4. washThe suspension is washed with H2O
5. extractionextracted with ethyl acetate
6. extractionThe organic extract
7. washis washed with brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered through a thin pad of hydrous magnesium silicate
10. customThe filtrate is evaporated
11. customthe residue triturated with diethyl ether-hexane