反应详情

500 mg of powdered molecular sieve (4 Å) and 113 mg (0.96 mmol) of N-methylmorpholine N-oxide are added to a solution of the crude product from example 18A in 2 ml of dry dichloromethane. 11 mg (0.03 mmol) of tetrapropylammonium perruthenate are then added to the reaction mixture, which is then stirred at RT for 1 h. The mixture is purified directly by chromatography on a silica gel fritte (mobile phase: gradient dichloromethane/ethanol 100:1→10:1). All product-containing fractions are combined, the solvent is removed on a rotary evaporator and the residue is purified further by another silica gel chromatography (mobile phase: gradient dichloromethane/ethanol 200:1→5:1).

1. customThe mixture is purified directly by chromatography on a silica gel fritte (mobile phase: gradient dichloromethane/ethanol 100:1→10:1)
2. customthe solvent is removed on a rotary evaporator
3. customthe residue is purified further by another silica gel chromatography (mobile phase: gradient dichloromethane/ethanol 200:1→5:1)