反应详情

温度

60 °C

5,6-Dichloro-3-methyl-2-(methylthio)benzimidazole (Int-k) (5.58 g, 0.022 mol) and 4.22 g methyl p-toluenesulfonate were mixed with 10 ml xylenes and heated to 124°-136° C. for 5 hrs. Upon cooling to 60° C., acetone was added to cover and slurry. The product was collected by filtration and reslurried in acetone. Filtration and drying yielded 3.14 g, mp 152°-156° C. The product was again slurried with acetone overnight to give 2.38 g, mp 152°-155° C., which NMR indicated was contaminated with some unreacted starting material.

1. temperatureheated to 124°-136° C. for 5 hrs
2. filtrationThe product was collected by filtration
3. filtrationFiltration
4. customdrying
5. customyielded 3.14 g, mp 152°-156° C
6. customto give 2.38 g, mp 152°-155° C., which NMR