反应详情

Dissolve 3,4-difluoronitrobenzene (2.0 g, 12.6 mmol) in acetonitrile (35 mL) and add piperazine-1-carboxylic acid tert-butyl ester (4.7 g, 25.2 mmol). Heat the mixture at reflux for 16 h. Cool the mixture to room temperature and concentrate in vacuo. Partition the residue between dichloromethane (75 mL) and water (75 mL), separate the organic portion and extract the aqueous portion with dichloromethane (2×25 mL). Combine the organics and dry (Na2SO4), filter, and concentrate in vacuo to give 2.83 g (72%) of the title compound. MS/ES m/z 270.2 [M-tertBu+H]+.

1. temperatureHeat the mixture
2. temperatureat reflux for 16 h
3. concentrationconcentrate in vacuo
4. customPartition the residue between dichloromethane (75 mL) and water (75 mL)
5. customseparate the organic portion
6. extractionextract the aqueous portion with dichloromethane (2×25 mL)
7. dry with materialCombine the organics and dry (Na2SO4)
8. filtrationfilter
9. concentrationconcentrate in vacuo