反应详情

温度

0 °C

2-Carbamoylmethoxyphenoxyacetamide (Intermediate A64, 112 g, 0.50 mol) was added portion wise over 15 min to rapidly stirred chlorosulfonic acid (582.5 g, 5.0 mol) and cooled to 0° C. Then dichloromethane (120 mL) was added, and the mixture was heated in a 60°-70° C. bath for 3 hr. The mixture was slowly poured into 1.5 Kg of crushed ice, and water (500 mL) was added. The resulting solid was collected, washed with water and acetone, resuspended in acetone, filtered, washed with acetone, and air dried to yield 125 g (77%) of the title compound.

1. temperaturethe mixture was heated in a 60°-70° C. bath for 3 hr
2. additionwas added
3. customThe resulting solid was collected
4. washwashed with water and acetone
5. filtrationfiltered
6. washwashed with acetone, and air
7. customdried