反应详情

温度

0 °C

In a 50 mL 3-neck RBF, 3-nitroaniline 5 (5.0 g) in THF (40 mL) and (BOC)2O (7.89 g) was charged and cooled to 0° C. DMAP (6.09 g) was added portion-wise into the reaction mixture and reaction mixture was warmed to room temperature and stirred at room temperature for 5 hr. The reaction was monitored on TLC using hexane:ethyl acetate (5:5) as mobile phase. After completion of the reaction, the reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with 50 mL brine solution, dried over sodium sulfate and concentrated completely under reduced pressure at 40° C. Crude material was purified by using column chromatography. Product was eluted with 4% ethyl acetate in hexane and concentrated to give 7.1 g of tert-butyl(3-nitrophenyl)carbamate.

1. custominto the reaction mixture and reaction mixture
2. temperaturewas warmed to room temperature
3. customAfter completion of the reaction
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with 50 mL brine solution
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated completely under reduced pressure at 40° C
8. customCrude material was purified
9. washProduct was eluted with 4% ethyl acetate in hexane
10. concentrationconcentrated