反应详情

1,1-carbonyldiimidazole (0.36 g, 2.23 mmol) was added to a solution of tert-butyl 2-(2-aminophenylamino)ethylcarbamate (0.56 g, 2.23mmol) in dichloromethane (15 mL) and stirred at rt overnight. Water (50 mL) was added and the mixture was extracted with dichloromethane (3×50 mL). The combined organic layers were washed with brine (50 mL), dried over anhydrous sodium sulfate and filtered. The solvent was removed and the product was purified by column chromatography eluting with ethyl acetate/hexane (1:3) to give the title compound (230 mg, 37%).

1. extractionthe mixture was extracted with dichloromethane (3×50 mL)
2. washThe combined organic layers were washed with brine (50 mL)
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. customThe solvent was removed
6. customthe product was purified by column chromatography
7. washeluting with ethyl acetate/hexane (1:3)