反应详情

温度

80 °C

To a solution of 4-carbobenzyloxypiperazine-2-carboxylic acid, copper chelate in 750 ml water was added ethylenediaminetetracetic acid, disodium salt, dihydrate (7.9 g, 21 mmol) and the blue mixture was heated to 80° C. for 3 h. The reaction mixture was cooled to rt and concentrated to dryness. The blue residue was dissolved in 100 ml DMSO. 2,4-dichloronitrobenzene (6.66 g, 35 mmol) and triethyl amine (20 ml, 143 mmol) were added and the solution was heated to 60° C. for 16 h. The dark reaction mixture was cooled to rt. Concentrated HCl was added to pH=3. The solution was then diluted with 500 ml water and the aqueous layer was extracted with ethyl acetate. The combined organics were washed with water, dried over MgSO4 and concentrated to afford 4-carbobenzyloxy-l-(4-chloro-2-nitrophenyl)piperazine-2-carboxylic acid as a yellow residue used directly in the next step.

1. temperatureThe reaction mixture was cooled to rt
2. concentrationconcentrated to dryness
3. dissolutionThe blue residue was dissolved in 100 ml DMSO
4. temperaturethe solution was heated to 60° C. for 16 h
5. customThe dark reaction mixture
6. temperaturewas cooled to rt
7. extractionthe aqueous layer was extracted with ethyl acetate
8. washThe combined organics were washed with water
9. dry with materialdried over MgSO4
10. concentrationconcentrated