反应详情

Methyl 13-cyclohexyl-6-formyl-5-methyl-6,7-dihydro-5H-indolo[1,2-d][1,4]benzodiazepine-10-carboxylate was dissolved in MeOH (0.08 M) and HOAc was added. Tert-butyl[(3-{methyl[2(methylamino)ethyl]amino}propyl)sulfonyl]carbamate (1.5 eq. prepared as described in Example 15, Steps 1-3) was added and the mixture was stirred for 5 min. NaCNBH3 (1.5 eq.) was added and the mixture was stirred for 6 h. All volatiles were evaporated and the residual material was dissolved in EtOAc. The solution was extracted with sat. aq. NH4Cl, sat. aq. NaHCO3 and brine. After drying over Na2SO4 all volatiles were evaporated in vacuo. A yellow amorphous solid was obtained which was used without further purification in the next reaction (60%). (ES+) m/z 711 (M+H)+.

1. stirringthe mixture was stirred for 6 h
2. customAll volatiles were evaporated
3. dissolutionthe residual material was dissolved in EtOAc
4. extractionThe solution was extracted with sat. aq. NH4Cl, sat. aq. NaHCO3 and brine
5. dry with materialAfter drying over Na2SO4 all volatiles
6. customwere evaporated in vacuo
7. customA yellow amorphous solid was obtained which
8. customwas used without further purification in the next reaction (60%)