反应详情

温度

145 °C

A glass pressure vessel was charged with 5.5 grams (0.03 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole, 7.4 grams (0.06 mole) phenyl isocyanate and 50 milliliters benzene. A magnetic stirring bar was added and the vessel sealed. The stirred reaction mixture was heated at 145° C. for 1.5 hours and then allowed to cool to room temperature where a urea by-product precipitates. The by-product was removed by filtration and the filtrate concentrated in vacuo to leave 9.0 grams of crude product. Trituration with cold methanol gave 2.8 grams (24% yield) of pure product; m.p. 170° C.

1. additionA magnetic stirring bar was added
2. customthe vessel sealed
3. customThe stirred reaction mixture
4. customprecipitates
5. customThe by-product was removed by filtration
6. concentrationthe filtrate concentrated in vacuo
7. customto leave 9.0 grams of crude product