反应详情

温度

130 °C

A mixture of methyl 6-[(4-tert-butylphenyl)sulfonyl]-2-(trifluoromethyl)-6,11-dihydro-5H-pyrido-[2,3-b][1,5]benzodiazepine-8-carboxylate (90 mg, intermediate 56), water (0.63 mL), conc. HCl (1.25 mL), and glacial acetic acid (2.0 mL) was heated at 130° C. for 2 h. After cooling to rt, 4N aqueous NaOH was added until pH=6. The reaction mixture was extracted with DCM (3×), and the extracts were dried, filtered, and concentrated to provide the title compound. LC/MS: m/e 506.1 (M+H)+. 1H NMR (500 MHz, CDCl3): δ 8.12 (1H, s), 7.79 (1H, dd, J=8.5, 1.6 Hz), 7.49 (1H, d, J=7.5 Hz), 6.99 (3H, m), 6.79 (3H, m), 4.45-4.70 (2H, br), 1.11 (9H, s).

1. temperatureAfter cooling to rt
2. extractionThe reaction mixture was extracted with DCM (3×)
3. customthe extracts were dried
4. filtrationfiltered
5. concentrationconcentrated