反应详情

To a solution of 406 (39.8 mg, 0.1 mmol) in THF (2 ml) was added DIBAL-H (1.0 M in CH2Cl2, 0.2 ml, 0.2 mmol) at −78° C. The reaction mixture was stirred at this temperature for 6 h, then at 0° C. for 2 h, quenched with water (0.1 ml). The solid was filtered off, and the filtrate was concentrated. The residue was purified by preparative TLC to give the title compound (22.8 mg, 64%) as a brown solid (2.5% MeOH—CH2Cl2). LCMS Found: (M+H)+=357.

1. waitat 0° C. for 2 h
2. customquenched with water (0.1 ml)
3. filtrationThe solid was filtered off
4. concentrationthe filtrate was concentrated
5. customThe residue was purified by preparative TLC