反应详情

温度

150 °C

A mixture of tert-butyl 3-iodoazetidine-1-carboxylate (1 g, 3.53 mmol), 4-aminophenylboronic acid (630 mg, 4.59 mmol), NiI2 (66 mg, 0.212 mmol), NaHMDS (1.94 g, 10.6 mmol), (1R,2S)-2-aminocyclohexanol (24 mg, 0.212 mmol) in isopropanol (8 mL) was stirred at 150° C. in microwave for 2 h. It was then evaporated and the residue was dissolved with water and ethyl acetate. The water phase was separated and extracted with ethyl acetate. The combined extracts were dried over sodium sulfate and concentrated under reduced pressure. The residue was purified with column chromatography to give 298a (360 mg, 40%). MS: [M+H]+ 249.

1. customIt was then evaporated
2. dissolutionthe residue was dissolved with water and ethyl acetate
3. customThe water phase was separated
4. extractionextracted with ethyl acetate
5. dry with materialThe combined extracts were dried over sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified with column chromatography