反应详情

温度

100 °C

(E)-3-(2-Amino-4-chlorophenyl)-acrylic acid methyl ester (Carling, Robert W.; et al. J. Med. Chem. (1993), 36(22), 3397-408) (3.3 g, 15.6 mmol) in THF (63 ml) was combined with (BOC)2O (6.8 g, 31.2 mmol) and refluxed for 4 hours. THF was evaporated and a second portion of (BOC)2O added (6.8 g, 31.2 mmol). The mixture was heated to 100° C. for 18 hours. Recrystallisation from TBME/hexanes rendered the title compound as colorless crystals (4.6 g; 94%).

1. temperaturerefluxed for 4 hours
2. customTHF was evaporated
3. additiona second portion of (BOC)2O added (6.8 g, 31.2 mmol)
4. customRecrystallisation from TBME/hexanes