反应详情

2-Hydroxybenzaldehyde (25; 1.2 g, 9.8 mmol), N-Boc-3-(methylsulfonyloxy)pyrrolidine (29; 2.6 g, 9.8 mmol), K2CO3 (2.0 g, 14.7 mmol) and tetrabutyl ammonium iodide (300 mg, cat) in CH2Cl2 (20 mL) was stirred at 70-80° C. for 18 h. DMF was removed by concentration under reduced pressure. The resulting residue was diluted with EtOAc (100 mL), washed with water (50 mL), dried (MgSO4) and concentrated under reduced pressure. The resulting residue was purified by chromatography (pentane:EtOAc=1:10) to afford 676 mg of tert-butyl 3-(2-formylphenoxy)pyrrolidine-1-carboxylate 30 as an oil (yield: 23%).

1. customDMF was removed by concentration under reduced pressure
2. additionThe resulting residue was diluted with EtOAc (100 mL)
3. washwashed with water (50 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by chromatography (pentane:EtOAc=1:10)