反应详情

温度

100 °C

Intermediate 2 (0.45 g, 2.0 mmol), methyl azetidine-3-carboxylate hydrochloride (0.61 g, 4.0 mmol), and cesium carbonate (2.0 g, 6.0 mmol) were combined in degassed DMF (10 mL) and heated at 100° C. for 14 h. The mixture was cooled to room temperature and treated with iodomethane (0.13 mL, 2.0 mmol). After stirring for 1 h, the mixture was poured into sodium bicarbonate (200 mL, aqueous saturated) and extracted with ethyl acetate (2×100 mL). The combined organic extracts were dried with sodium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel chromatography (0-100% EtOAc/hexanes), providing 107-1 as an off-white solid. MS: m/z=303.3 (M+H).

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with ethyl acetate (2×100 mL)
3. dry with materialThe combined organic extracts were dried with sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by silica gel chromatography (0-100% EtOAc/hexanes)