反应详情

A solution of 3-(4-chloro-phenyl)-2-(2-chloro-phenyl)-5-isopropyl-4,5-dihydro-2H-pyrrolo[3,4-c]pyrazol-6-one 3A-1 (7 mg, 0.018 mmol) and BH3THF (166 ml, 166 mmol) was stirred at room temperature for 1 hour and at 50° C. for 17 hours. After the reaction mixture was cooled to room temperature, MeOH (5 ml) was added. The reaction mixture was heated under reflux for 2 h, cooled to room temperature, and concentrated in vacuo. The residue was diluted with 4 M HCl/dioxanes (1 ml) and concentrated under vacuum. The residue was dissolved in CH2Cl2 and hexanes were added to precipitate 8A-1 as a colorless solid (2 mg, 27%): +APCI MS (M+H) 372.5; 1H NMR (CD3OD): δ 7.59-7.43 (m, 4H), 7.38 (d, 2H), 7.20 (d, 2H), 4.80-4.65 (m, 2H), 3.91-3.82 (m, 1H), 3.68-3.55 (m, 2H), 1.52 (d, 6H).

1. temperatureThe reaction mixture was heated
2. temperatureunder reflux for 2 h
3. temperaturecooled to room temperature
4. concentrationconcentrated in vacuo
5. additionThe residue was diluted with 4 M HCl/dioxanes (1 ml)
6. concentrationconcentrated under vacuum
7. dissolutionThe residue was dissolved in CH2Cl2
8. additionhexanes were added
9. customto precipitate 8A-1 as a colorless solid (2 mg, 27%)