反应详情

To a stirred solution of phenyl [1-(2-hydroxyethyl)-5-(tritylamino)-1H-pyrazol-4-yl]carbamate (1 g) in N,N-dimethylformamide (10 ml) were added di-tert-butyl (2-amino-1,3-propanediyl)biscarbamate (631 mg) and triethylamine (0.83 ml), and the mixture was stirred at room temperature for 3 hours. Water was added to the reaction mixture and the whole mixture was extracted with ethyl acetate. The extract was washed with water and brine and dried over anhydrous magnesium sulfate. Concentration under reduced pressure gave a crude product, which was triturated with ethyl acetate-diisopropyl ether (1:3). The resulting solid was collected by filtration to give di-tert-butyl {2-[({[1-(2-hydroxyethyl)-5-(tritylamino)-1H-pyrazol-4-yl]amino}carbonyl)amino]-1,3-propanediyl}biscarbamate (435 mg).

1. extractionthe whole mixture was extracted with ethyl acetate
2. washThe extract was washed with water and brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationConcentration under reduced pressure
5. customgave a crude product, which
6. customwas triturated with ethyl acetate-diisopropyl ether (1:3)
7. filtrationThe resulting solid was collected by filtration