反应详情

3-(2-hydroxyethyl)-2-[2-(4-isopropylsulfonylphenyl)-5-trityl-pyrrolo[2,3-b]pyrazin-7-yl]isoindolin-1-one (58 mg, 0.08068 mmol) dissolved in DCM (2 mL) under N2 and Et3SiH (64.44 μL, 0.4034 mmol) then TFA (300 μL) added. Reaction mixture stirred overnight, then concentrated and residue azeotroped with DCM (×3). Purified by hplc to give the title compound as a pale yellow solid (19.3 mg, 50%); 1H NMR (400 MHz, DMSO) 1.03 (6H, d), 1.72-1.79 (1H, m), 2.00-2.15 (1H, m), 3.00-3.09 (1H, m), 3.32 (1H, sep), 4.28 (1H, t), 5.82-5.85 (1H, m), 7.42 (1H, t), 7.57 (1H, t), 7.65 (2H, d), 7.80 (2H, d), 8.21 (1H, s), 8.32 (2H, d), 8.93 (1H, s), 12.30 (1H, brs); MS (ES+) 477.0.

1. customReaction mixture
2. concentrationconcentrated
3. customresidue azeotroped with DCM (×3)
4. customPurified by hplc