反应详情

Bis(1,1-dimethylethyl)2-[1-hydroxy-2-phenyl-1-(phenylmethyl)ethyl]-1,4-piperazinedicarboxylate (2.0 g, 4.0 mmol) was dissolved in N,N-dimethylformamide (20 mL). 60% Sodium hydride (0.19 g, 4.8 mmol) was added thereto, and the mixture was stirred at room temperature for 6 hours. The resulting mixture was extracted with ethyl acetate, washed with a 0.5 M aqueous sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. To the residue was added diisopropyl ether, and the obtained crystals were collected by filtration and washed with diisopropyl ether to obtain the title compound (1.4 g, yield 82%).

1. extractionThe resulting mixture was extracted with ethyl acetate
2. washwashed with a 0.5 M aqueous sodium hydrogen carbonate solution
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. additionTo the residue was added diisopropyl ether
6. filtrationthe obtained crystals were collected by filtration
7. washwashed with diisopropyl ether