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With dmap; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; In dichloromethane; at 40℃; for 1.5h;
A suspension of <strong>[1214196-85-6]1-Boc-piperazine-2-carboxylic acid</strong> (9, 2.0 g, 8.69 mmol), EDCI (1.99 g, 10.42 mmol) and DMAP (0.32 g,2.61 mmol) in MeOH/CH2Cl2 (1:1) was stirred at 40 C for 1.5 hr, then the resulting solution was cooled down to room temperature and stirred for another 4 hrs. After removing the solvent, the residue was dissolved in CH2Cl2. The solution was washed with H2O (50 mL x 3). The combined aqueous was re-extracted with CH2Cl2 (40 mL x 3). All of the organics were combined, washed with 1 N NaHCO3 (50 mL x 3) and brine, and finally dried over Na2SO4. The product, a colorless liquid, was purified via flash chromatography, eluted with CH2Cl2 then 10% MeOH/CH2Cl2. Rf= 0.7 (10% MeOH/CH2Cl2, stained by phosphomolybdic acid (PMA)); yield - 84%
79%
With dmap; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; In dichloromethane; at 20 - 40℃; for 21.5h;Inert atmosphere;
A 50 mL rb flask equipped with an air condenser, rubber septum and a magnetic stir bar was set under Ar atmosphere and charged with 500 mg of 1 -(/tv7-b utoxy carbonyl)piperazine-2- carboxylic acid (2.17 mmol, 1 equiv.), 80.0 mg of DMAP (0.651 mmol, 0.3 equiv.), 500 mg of EDCI (2.61 mmol, 1.2 equiv.), 10 mL of CH2CI2 and 3 mL of dry methanol. The reaction mixture was stirred at 40 C for 1.5 h and then the reaction was allowed to cool to rt. After stirring for 20 h, the reaction mixture was concentrated and the residue was dissolved in CH2CI2. The CH2CI2 solution was washed with water (3x). The water solutions were combined and the product was back-extracted with CH2CI2 (3x). Then the combined organics were washed with sat. NaHC03 solution, brine and dried over Na2S04. The crude product (661 mg) was purified on silica gel column using 0 to 5 % MeOH in CH2CI2 as eluent affording 419 mg (79 %) of the product 41 as a colorless oil.
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