反应详情

温度

150 °C

A mixture of 2 g (11.6 mmol) 5-chloro-2-nitro-phenylamine, 2.14 g (11.6 mmol) piperazine-1-carboxylic acid tert-butyl ester and 1.3 g (11.6 mmol) 1,4-diazo-bicyclo[2.2.2]octane in 20 ml DMSO was heated to 150° C. for 16 h. The mixture was poured onto 200 ml water and extracted with 250 ml ethyl acetate. The emulsion was filtered through decalite and the aqueous phase was extracted with 2×200 ml. The combined organic phases were washed with 2×100 ml water, dried with MgSO4 and evaporated to dryness. The residue was purified with column chromatography on silica eluting with ethyl acetate/hexane to yield the title compound as a yellow solid. MS(ISP): 321.2 (M−H)−.

1. extractionextracted with 250 ml ethyl acetate
2. filtrationThe emulsion was filtered through decalite
3. extractionthe aqueous phase was extracted with 2×200 ml
4. washThe combined organic phases were washed with 2×100 ml water
5. dry with materialdried with MgSO4
6. customevaporated to dryness
7. customThe residue was purified with column chromatography on silica eluting with ethyl acetate/hexane