反应详情

温度

55 °C

A mixture of 2.5 g of (2-methoxycarbonylbenzyl)sulfonamide, 21.5 g of 4,6-dimethoxy-2-isothiocyanatopyrimidine and 15.1 g of anhydrous potassium carbonate in 400 ml of acetone is stirred for 8.5 hours at 55° C., and then filtered to collect precipitated crystals. To the filtrate, further 2 g of anhydrous potassium carbonate is added and stirred for 2 hours at 60° C. The precipitated crystals are collected. The combined crystals are suspended in 1.5 of water and adjusted to pH 2 with hydrochloric acid. After stirring the mixture for an hour, the crystals are collected by filtration, washed with water, dried and recrystallized from acetonitrile to give 35.9 g of the title compound, as white powder.

1. filtrationfiltered
2. customto collect
3. customprecipitated crystals
4. additionTo the filtrate, further 2 g of anhydrous potassium carbonate is added
5. stirringstirred for 2 hours at 60° C
6. customThe precipitated crystals are collected
7. stirringAfter stirring the mixture for an hour
8. filtrationthe crystals are collected by filtration
9. washwashed with water
10. customdried
11. customrecrystallized from acetonitrile