反应详情

1.09 g of 4-oxotetrahydropyran-3-sulfonamide were dissolved in THF, 0.23 g of sodium borohydride was added and the mixture was stirred at room temperature for 18 hours. The mixture was then adjusted to pH=2 with hydrochloric acid and concentrated under reduced pressure. The residue, bound to 8 g of Celite, was purified by means of a silica gel column (50 g): solvent A: dichloromethane, B: methanol, gradient: 0 min 3% B, 3 min 3% B, 5 min 5% B, 35 min 10% B, 44 min 10% B; flow rate 20 ml/min; detection: 220 nm, fraction size: 20 ml. After removal of the solvent under reduced pressure, the product was thus obtained with impurities. The residue (615 mg) was used further without further workup.

1. concentrationconcentrated under reduced pressure
2. customwas purified by means of a silica gel column (50 g)
3. custom0 min 3% B, 3 min 3% B, 5 min 5% B, 35 min 10% B, 44 min 10% B
4. customAfter removal of the solvent under reduced pressure
5. customthe product was thus obtained with impurities