反应详情

温度

50 °C

A mixture of 4-tert-butyl-phenylamine (5.8 mL, 36.5 mmol), 2-amino-benzoic acid (5.0 g, 36.5 mmol), TBTU (12.9 g, 40.2 mmol) and DIEA (6.7 mL, 40.2 mmol) in 5 mL of DMF was heated (50° C.) for 12 h in a sealed tube. The mixture was diluted with EtOAc and the aqueous layer was extracted with EtOAc. The combined organic layers were dried over Na2SO4, filtered and concentrated in vacuo. The crude material was purified by flash chromatography (SiO2, 20% EtOAc/hexane) and crystallized from EtOH:H2O (3:1) to afford a yellow solid. MS (ES+): 269.4. (M+H)+. Calc'd for C17H20N2O-268.35.

1. extractionthe aqueous layer was extracted with EtOAc
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by flash chromatography (SiO2, 20% EtOAc/hexane)
6. customcrystallized from EtOH:H2O (3:1)
7. customto afford a yellow solid