Dichloromethane → HCID 13493680, compound

Participants

Reaction Conditions

Reaction Steps

To a stirred mixture of the product of Example 46d (700 mg, 5.0 mmol) and sodium bicarbonate (420 mg, 5.0 mmol) in dichloromethane (10 mL) at 0° C. under argon was added Dess-Martin periodinane (3.14 g, 7.4 mmol). The reaction mixture was stirred at 0° C. for 2 hours and then slowly warmed to room temperature. The mixture was concentrated under reduced pressure and the residue purified by column silica gel chromatography to give the title compound as a colorless oil (600 mg, Yield: 85% yield). Rf=0.8 (10:1) petroleum ether/:ethyl acetate); 1H NMR (400 MHz, CDCl3) δ 9.81 (d, J=2.4 Hz, 1H), 2.10-2.05 (m, 1H), 1.50-1.24 (m, 8H), 1.13 (s, 3H), 0.99 (s, 3H) ppm.

Provenance & Evidence