反应详情

To a stirred suspension of 1.4 g of 2-amino-4-methoxy-6-methylpyrimidine in 30 ml of anhydrous methylene chloride was added at ambient temperature 2.4 g of 2-methoxycarbonylbenzenesulfonylisocyanate. After stirring for 16 hours, the foregoing mixture was filtered to remove unreacted amine, and the filtrate evaporated at temperatures up to 40° and reduced pressure. The resultant residue was stirred in 25 ml of water, the pH adjusted to 10 by the addition of 50% sodium hydroxide and the solution filtered. Acidification of the filtrate to pH 3 with hydrochloric acid caused precipitation of the desired product which was removed by filtration and dried to yield 0.8 g of product melting at 173°-179°. It showed infrared absorption peaks at 1720, 1680, 1630 and 1550 cm-1, consistent for N-[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]-2-methoxycarbonylbenzenesulfonamide.

1. filtrationthe foregoing mixture was filtered
2. customto remove unreacted amine
3. customthe filtrate evaporated at temperatures up to 40°
4. stirringThe resultant residue was stirred in 25 ml of water
5. additionthe pH adjusted to 10 by the addition of 50% sodium hydroxide
6. filtrationthe solution filtered
7. customprecipitation of the desired product which
8. customwas removed by filtration
9. customdried