反应详情

温度

0 °C

Trichloroacetyl isocyanate (10 g, 53 mmol) was added dropwise to the solution of 2-amino-thiophene-3-carboxylic acid amide (3.8 g, 26.5 mmol) in pyridine (110 mL) at 0° C. The resulting reaction mixture was stirred at 0° C. The temperature of the reaction mixture was raised to room temperature over a 3 h period until LC-MS showed no remaining starting material. Diethyl ether (100 mL) was added to the reaction mixture and the resulting precipitate was filtered and dried under vacuum to give the above titled compound as a light grey solid (8.7 g, 26.3 mmol, 99% yield).

1. customThe resulting reaction mixture
2. temperatureThe temperature of the reaction mixture was raised to room temperature over a 3 h period until LC-MS
3. filtrationthe resulting precipitate was filtered
4. customdried under vacuum