反应详情

温度

40 °C

2,3,5-Tribromo-4-methoxy-aniline (4.72 g, 13.1 mmol) was dissolved in acetone (150 mL) and ethoxycarbonyl isothiocyanate (1.63 mL, 14.4 mmol) was added. The solution was heated to 40° C. After 20 minutes a pale yellow precipitate had formed. The viscous mixture was cooled to rt and stirred at rt overnight. The solvent was removed under reduced pressure. Cyclohexane (˜150 mL) was added to the residue and the suspension sonicated. The solid was collected by filtration through a PTFE filter to give an off-white fluffy solid which was dried in the vacuum oven (40° C.) to afford the desired compound as an off-white solid, 6.00 g (93%). m/z: 488.78/490.80/492.75/494.80 [M+H]+.

1. customAfter 20 minutes a pale yellow precipitate had formed
2. temperatureThe viscous mixture was cooled to rt
3. customThe solvent was removed under reduced pressure
4. additionCyclohexane (˜150 mL) was added to the residue
5. customthe suspension sonicated
6. filtrationThe solid was collected by filtration through a PTFE
7. filtrationfilter
8. customto give an off-white fluffy solid which
9. customwas dried in the vacuum oven (40° C.)