反应详情

温度

80 °C

To a solution of (Z)-ethyl 3-((2-amino-2-oxoethyl)amino)-3-(2-(2-hydroxyethoxy)phenyl)acrylate (1.0 g, 3.25 mmol) in tetrahydrofuran (15 mL) was added trimethylsilyl isothiocyanate (1.7 g, 12.9 mmol), and the mixture was stirred at 80° C. for 18 hours. The reaction mixture was cooled to room temperature, poured into a flask containing water and extracted with CH2Cl2 (3×100 mL). The combined organic layers were dried and concentrated under reduced pressure to give a yellow solid, which was purified by flash chromatography (2-5% MeOH:CH2Cl2) to give the title compound (330 mg, 31.7%) as a yellow solid.

1. temperatureThe reaction mixture was cooled to room temperature
2. additionpoured into a flask
3. extractionextracted with CH2Cl2 (3×100 mL)
4. customThe combined organic layers were dried
5. concentrationconcentrated under reduced pressure
6. customto give a yellow solid, which
7. customwas purified by flash chromatography (2-5% MeOH:CH2Cl2)