反应详情

To a stirred solution of 2,3-dihydrospiro[indene-1,4′-piperidine] (0.4 g, 1.78 mmol) in DMF (12 mL) is added Cs2CO3 (1.4 g, 4.4 mmol) and [4-(bromomethyl)phenyl]methanol (0.36 g, 1.78 mmol) and the reaction mixture is stirred overnight at room temperature. The reaction mixture is poured into cold water and extracted with EtOAc (3×50 mL). The combined organic layer is washed with brine solution, dried over Na2SO4, and concentrated under vacuum. The crude material is purified by silica gel chromatography (gradient DCM/MeOH 8/2) to give the title compound (0.6 g, 98%). ESI/MS m/z 308.40 (M+H)+.

1. extractionextracted with EtOAc (3×50 mL)
2. washThe combined organic layer is washed with brine solution
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under vacuum
5. customThe crude material is purified by silica gel chromatography (gradient DCM/MeOH 8/2)