反应详情

A solution of methyl-2-(tert-butoxycarbonyl)-3-(7-methyl-2-[{2-[trimethylsilyl]ethoxy}methyl]-2H-indazol-5-yl)acrylate (3.7 g, 8.0 mmol) in methanol (20 mL) was flushed with nitrogen (2×), and treated with palladium (10% on charcoal, 0.37 g). The flask was flushed with hydrogen and was shaken in a parr apparatus overnight at 60 psi. The reaction was flushed with nitrogen, filtered through celite, and concentrated. Column chromatography gave 2.3 g (63%). 1H-NMR (CDCl3, 500 MHz) δ −0.03 (s, 9H), 0.92-0.97 (m, 2H), 1.41 (s, 9H), 2.59 (s, 3H), 3.00-3.17 (m, 2H), 3.59-3.67 (m, 2H), 3.71 (s, 1H), 4.54-4.64 (m, 1H), 4.92-5.01 (m, 1H), 5.71 (s, 2H), 6.82 (s, 1H), 7.12-7.19 (m, 2H), 8.01 (s, 1H). Mass spec.: 464.29 (MH)+.

1. customThe flask was flushed with hydrogen
2. customThe reaction was flushed with nitrogen
3. filtrationfiltered through celite
4. concentrationconcentrated
5. customColumn chromatography gave 2.3 g (63%)