反应详情

A solution of 97.7 mg (0.23 mmol) of Dess Martin periodinane reagent (Aldrich) in 1 ml of DCM is slowly added dropwise to a solution of 56 mg (0.21 mmol) of methyl 2-benzyloxycarbonylamino-3-hydroxy-2-methylpropionate in 1 ml of DCM, and the mixture is left to stir at room temperature for 30 min. 5 ml of diethyl ether and a mixture of 4 ml of saturated NaHCO3 and 0.36 g of Na2S2O3.5H2O are then added to the solution. It is stirred for 15 min until the solid has dissolved, and then the ether phase is washed with saturated NaHCO3 and water, dried over MgSO4 and concentrated in vacuo. The crude product is purified by chromatography on 4 g of SiO2 with EtOAc/heptane (gradient 0-50%). 40 mg of the desired aldehyde are obtained.

1. waitthe mixture is left
2. additionare then added to the solution
3. stirringIt is stirred for 15 min until the solid
4. dissolutionhas dissolved
5. washthe ether phase is washed with saturated NaHCO3 and water
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo
8. customThe crude product is purified by chromatography on 4 g of SiO2 with EtOAc/heptane (gradient 0-50%)