反应详情

Ethyl ether (15 ml) and an excess of anhydrous sodium carbonate were added to a mixture in water of 0.13 g (0.5 mmole) of 5-[(dimethylamino)methyl]-2-furanmethanethiol oxalate (1:1), sodium dithionite (0.05 g) and anhydrous sodium carbonate (0.15 g). The mixture was filtered and the filtrate was evaporated under vacuum. 0.087 g (0.5 mmole) of N-(2-hydroxyethyl)-alpha-(nitromethylene)-1-aziridinemethaneamine and 4 ml of methanol were added to the residue. The mixture was evaporated to dryness and the residue was heated to 95°-100° C. for 1 hour and chromatographed over silica (methanol-0.88 NH3 ; 79:1). The appropriate eluate was evaporated under vacuum to give 0.12 g of N-[2-[[(5-[(dimethylamino)methyl]-2-furanyl)methyl]thio]ethyl]-N'-(2-hydroxyethyl)-2-nitro-1,1-ethenediamine having the same properties as the product prepared according to Example 1, paragraph (a).

1. filtrationThe mixture was filtered
2. customthe filtrate was evaporated under vacuum
3. customThe mixture was evaporated to dryness
4. temperaturethe residue was heated to 95°-100° C. for 1 hour
5. customchromatographed over silica (methanol-0.88 NH3 ; 79:1)
6. customThe appropriate eluate was evaporated under vacuum