反应详情

A mixture of the above aldehyde and sodium borohydride (400 mg, 10 mmol) in EtOH (50 mL) is stirred at room temperature for 1 hour. After evaporation of EtOH, EtOAc (40 mL) and water (40 mL) are added to the residue. The organic layer is separated, washed once with 1 N NaOH, 1N HCl and brine, dried (Na2SO4) and concentrated. The residue is chromatographed on silica gel (1:1 hexane:EtOAc) to give (2,6-dichloro-3-hydroxymethyl-pyridin-4-yl)-pyrrolidin-1-yl-methanone.

1. customAfter evaporation of EtOH, EtOAc (40 mL) and water (40 mL)
2. additionare added to the residue
3. customThe organic layer is separated
4. washwashed once with 1 N NaOH, 1N HCl and brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customThe residue is chromatographed on silica gel (1:1 hexane:EtOAc)