反应详情

温度

80 °C

To a solution of dimethyl 2-aminoterephthalate (500 g, 2.39 mol) in CCl4 (4 L) at 60° C. was slowly added NCS (957 g, 7.17 mol). The reaction mixture was heated at 80° C. for 16 hours, cooled to room temperature and filtered. The solid was washed with dichloromethane (2×500 mL) and the combined organic solution was washed with 1 N NaOH (2×3 L), water (3 L) and brine (1 L). The mixture was dried over Na2SO4, and concentrated under reduced pressure to afford dimethyl 2-amino-3,5-dichloroterephthalate (645 g, yield: 97%) as a red oil. 1H NMR (400 MHz, DMSO-d6) δ 3.81 (s, 3H), 3.87 (s, 3H), 7.04 (s, 2H), 7.77 (s, 1H). LCMS (ESI) m/z: 210.0 [M+H+].

1. customat 60° C.
2. temperaturecooled to room temperature
3. filtrationfiltered
4. washThe solid was washed with dichloromethane (2×500 mL)
5. washthe combined organic solution was washed with 1 N NaOH (2×3 L), water (3 L) and brine (1 L)
6. dry with materialThe mixture was dried over Na2SO4
7. concentrationconcentrated under reduced pressure