反应详情

0.084 g of sodium hydride (60% pure in paraffin oil) was added to a suspension of 0.23 g of 2-amino-4-methoxy-6-methyl-1,3,5-triazine in 3 ml of dimethylacetamide (DMA) at room temperature to form a mixture. The mixture was stirred until the evolution of gas ended. A solution of 0.44 g of diphenyl carbonate in 1 ml of DMA was then slowly added dropwise at about 5° C., and the resulting mixture therefrom was stirred for 10 minutes. A solution of 0.68 g of methyl 2-aminosulfonyl-4-iodobenzoate (92.5% pure) in 2 ml of DMA was slowly added dropwise, to the resulting mixture, while cooled in an ice bath, to form a reaction mixture. When the reaction ended, the reaction mixture was then introduced into a solution of 30 ml of ice-water and 0.25 ml of concentrated hydrochloric acid, whereby a crude product separated out. The crude product which separated out was then purified by washing with a little water, methanol and diisopropyl ether and drying. The yield was 0.47 g (46% of theory).

1. customto form a mixture
2. stirringthe resulting mixture therefrom was stirred for 10 minutes
3. temperaturewhile cooled in an ice bath
4. customto form a reaction mixture
5. customseparated out
6. customThe crude product which separated out
7. customwas then purified
8. washby washing with a little water, methanol and diisopropyl ether
9. customdrying