反应详情

To a solution of 4-(9-benzenesulfonyl-3-bromo-6-cyano-9H-dipyrido[2,3-b;4′,3′-d]pyrrol-5-yloxy)piperidine-1-carboxylic acid tert-butyl ester (12.6 g, 20.6 mmol) in dichloromethane (36 mL) was added TFA (36 mL). After 1 hour at ambient temperature the reaction mixture was concentrated in-vacuo and the residue partitioned between saturated aqueous sodium carbonate solution (800 mL) and dichloromethane (2 L). The organic phase was separated, dried (Na2SO4), filtered and evaporated in-vacuo to afford the title compound as an off-white solid (8.8 g, 84%) which was used without further purification. 1H NMR (300 MHz, DMSO-d6): 9.46 (s, 1H), 8.90 (d, J=2.3 Hz, 1H), 8.64 (d, J=2.3 Hz, 1H), 8.23-8.22 (m, 2H), 7.78 (t, J=7.4 Hz, 1H), 7.64 (t, J=7.8 Hz, 2H), 4.85-4.85 (m, 1H), 3.17 (s, 1H), 3.00 (dt, J=13.0, 4.1 Hz, 2H), 2.50-2.49 (m, 2H obscured by solvent peak), 2.15-1.97 (m, 2H), 1.75-1.75 (m, 2H).

1. concentrationAfter 1 hour at ambient temperature the reaction mixture was concentrated in-vacuo
2. customthe residue partitioned between saturated aqueous sodium carbonate solution (800 mL) and dichloromethane (2 L)
3. customThe organic phase was separated
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customevaporated in-vacuo