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温度

0 °C

N-(3,4-Dichlorophenyl)piperazine-1-carboxamide (596 mg) and (2R)-1-BOC-piperazine-2-carboxylic acid (500 mg) were dissolved in N,N-dimethylformamide (30 ml) and stirred at 0° C. Triethylamine (0.61 ml) was added followed by PYBOP reagent (1.13 g). The mixture was allowed to warm to room temperature overnight, poured into saturated aqueous sodium bicarbonate (60 ml) and extracted with ethyl acetate (2×100 ml), adding a little water during the process to dissolve precipitated sodium bicarbonate. The combined organic extracts were treated with brine (100 ml), dried (sodium sulphate), concentrated in vacuo and adsorbed onto silica for purification by chromatography eluting with 0-15% methanol/dichloromethane. This gave the product as a white glass (710 mg).

1. temperatureto warm to room temperature overnight
2. extractionextracted with ethyl acetate (2×100 ml)
3. additionadding a little water during the process
4. dissolutionto dissolve
5. customprecipitated sodium bicarbonate
6. additionThe combined organic extracts were treated with brine (100 ml)
7. dry with materialdried (sodium sulphate)
8. concentrationconcentrated in vacuo
9. customadsorbed onto silica for purification by chromatography
10. washeluting with 0-15% methanol/dichloromethane