反应详情

The darkened mixture of 1.806 g (0.005 mol) of 11-[[[2-bromo-ethyl]amino]carbonyl]-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one, 0.992 g (0.005 mol) of 2-[(dipropylamino)-methyl]piperidine, 20 ml of anhydrous acetonitrile and 0.75 g (0.005 mol) of sodium iodide was refluxed for 4 hours with stirring under a nitrogen atmosphere. The mixture was left to cool, 50 ml of 10% aqueous potassium carbonate solution were added and the organic phase was separated off. The aqueous phase was extracted five times in all, with 10 ml aliquots of dichloromethane. The combined organic extracts were dried over sodium sulphate with the addition of animal charcoal and evaporated down in vacuo. The residue was purified by column chromatography on silica gel (30-60 microns) and using dichloromethane/cyclohexane/methanol/conc. ammonia 68/15/15/1 (v/v/v/v) as eluant. The corresponding eluates were evaporated down, the residue was recrystallised once from acetonitrile and dried in a vacuum dryer at 50° C. until a constant weight was obtained. 0.7 g (29% of theory) of colourless crystals were obtained, m.p. 163°-164° C., which were identical according to their mixed melting point, thin layer chromatogram and IR spectrum, to a preparation prepared according to Example 29.

1. temperaturewas refluxed for 4 hours
2. waitThe mixture was left
3. temperatureto cool
4. customthe organic phase was separated off
5. extractionThe aqueous phase was extracted five times in all, with 10 ml aliquots of dichloromethane
6. dry with materialThe combined organic extracts were dried over sodium sulphate with the addition of animal charcoal
7. customevaporated down in vacuo
8. customThe residue was purified by column chromatography on silica gel (30-60 microns)
9. customThe corresponding eluates were evaporated down
10. customthe residue was recrystallised once from acetonitrile
11. customdried in a vacuum dryer at 50° C. until a constant weight
12. customwas obtained
13. custom0.7 g (29% of theory) of colourless crystals were obtained
14. additionmixed melting point, thin layer chromatogram and IR spectrum
15. customto a preparation prepared