反应详情

温度

80 °C

A mixture of 3 g (14.78 mmol) of 5-bromo-2-nitropyridine, 5.5 g (29.56 mmol) of tert-butyl 1-piperazinecarboxylate, 5.46 g (14.78 mmol) of tetra-butylammonium iodine and 4.1 g (29.56 mmol) of potassium carbonate were placed in a flask. Dimethylsulfoxide (45 mL) is added and heat up to 80° C. for 24 hours. After cooling to room temperature, the precipitate is filtered and washed with ethyl acetate. Excess amount of water is added and extracted 4×. Dried with sodium sulfate and evaporated to give 2.7 g (59% yield) as a yellow solid. MS (ESI) m/z 309.1(M+1)

1. customwere placed in a flask
2. temperatureAfter cooling to room temperature
3. filtrationthe precipitate is filtered
4. washwashed with ethyl acetate
5. additionExcess amount of water is added
6. extractionextracted 4×
7. dry with materialDried with sodium sulfate
8. customevaporated
9. customto give 2.7 g (59% yield) as a yellow solid