反应详情

温度

2.5 °C

To a solution of 5-bromo-2-methoxy-4-methylbenzenesulfonic acid dihydrate (from (a), 125 g, 0.394 moles) in methanol (1.25 liters, 10 ml/g) was added 5% Palladium on carbon catalyst (12.5 g, 0.1 g/g) and the suspension was hydrogenated at 60° C. and 414 kPa (60 psi) for 16 hours. The reaction mixture was filtered over celite and concentrated to dryness. The crude product was slurried in dichloromethane (250 ml), cooled to 0-5° C. and the subtitle compound (67.5 g, 75% yield) isolated in two crops as a white crystalline solid

1. customwas hydrogenated at 60° C.
2. filtrationThe reaction mixture was filtered over celite and
3. concentrationconcentrated to dryness