反应详情

Methyl 13-cyclohexyl-6-(2,5,13,13-tetramethyl-9,9-dioxido-11-oxo-12-oxa-9-thia-2,5,10-triazatetradec-1-yl)-6,7-dihydro-5H-indolo[2,1-a][2]benzazepine-10-carboxylate was dissolved in DCM (0.1 M) and TFA (44 eq.) was added. After stirring at RT for 1 h all volatiles were evaporated in vacuo and the residual material was coevaporated three times with toluene. (MS (ES+): 595.6). The material was dissolved in MeOH (0.05 M) and 1 M KOH solution (10 eq.) was added and the mixture was stirred at 70° C. for 3 h. After cooling 1N hydrochloric acid was slowly added until neutral pH. The mixture was extracted three times with EtOAc, washed with water and brine. After drying the organic phase over Na2SO4 all volatiles were evaporated in vacuo. The residual material was used without further purification in the next reaction. (ES+) m/z 581 (M+H)+.

1. customwere evaporated in vacuo
2. dissolutionThe material was dissolved in MeOH (0.05 M)
3. stirringthe mixture was stirred at 70° C. for 3 h
4. additionwas slowly added until neutral pH
5. extractionThe mixture was extracted three times with EtOAc
6. washwashed with water and brine
7. dry with materialAfter drying the organic phase over Na2SO4 all volatiles
8. customwere evaporated in vacuo
9. customThe residual material was used without further purification in the next reaction