反应详情

2.59 g of potassium tert-butylate was added to a suspension of 2.85 g of 2-amino-4-methoxy-6-methyl-1,3,5-triazine in 40 ml of dimethylacetamide (DMA) at room temperature to form a first mixture. A solution of 4.94 g of diphenyl carbonate in 20 ml of DMA was then added dropwise to the first mixture at about 5° C. to form a second mixture. The second mixture was subsequently added dropwise to a solution of 5.00 g of methyl 2-aminosulfonyl-4-iodobenzoate (92.5% pure) in 15 ml of DMA at about 5° C., to form a third mixture. When the reaction ended, the third mixture was filtered over kieselguhr (®Celite). The filtrate was introduced into a solution of 200 ml of ice-water and 10 ml of concentrated hydrochloric acid, whereby the crude urea product separated out. The crude product which separated out was then purified by stirring with methanol and diisopropyl ether and dried. The yield was 4.50 g (66% of theory).

1. customto form a first mixture
2. customto form a second mixture
3. customto form a third mixture
4. filtrationthe third mixture was filtered over kieselguhr (®Celite)
5. additionThe filtrate was introduced into a solution of 200 ml of ice-water and 10 ml of concentrated hydrochloric acid, whereby the crude urea product
6. customseparated out
7. customThe crude product which separated out
8. customwas then purified
9. customdried